CN108264087A - A kind of single agents autoreaction, which prepares to have, aligns Nb2O5The method of nanometer rods - Google Patents
A kind of single agents autoreaction, which prepares to have, aligns Nb2O5The method of nanometer rods Download PDFInfo
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- CN108264087A CN108264087A CN201810216219.3A CN201810216219A CN108264087A CN 108264087 A CN108264087 A CN 108264087A CN 201810216219 A CN201810216219 A CN 201810216219A CN 108264087 A CN108264087 A CN 108264087A
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- nanometer rods
- noble metal
- aligns
- reaction kettle
- autoreaction
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Links
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 84
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 46
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims abstract description 38
- UKDIAJWKFXFVFG-UHFFFAOYSA-N potassium;oxido(dioxo)niobium Chemical compound [K+].[O-][Nb](=O)=O UKDIAJWKFXFVFG-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910000510 noble metal Inorganic materials 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 23
- 239000008367 deionised water Substances 0.000 claims abstract description 18
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 18
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 16
- 238000007789 sealing Methods 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 11
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052737 gold Inorganic materials 0.000 claims abstract description 5
- 239000010931 gold Substances 0.000 claims abstract description 5
- 239000011261 inert gas Substances 0.000 claims abstract description 5
- 239000010955 niobium Substances 0.000 claims description 55
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 24
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 18
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 17
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims description 16
- 229910001868 water Inorganic materials 0.000 claims description 11
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- BBKFSSMUWOMYPI-UHFFFAOYSA-N gold palladium Chemical compound [Pd].[Au] BBKFSSMUWOMYPI-UHFFFAOYSA-N 0.000 claims description 10
- 229910052763 palladium Inorganic materials 0.000 claims description 9
- 229910052697 platinum Inorganic materials 0.000 claims description 9
- 238000004064 recycling Methods 0.000 claims description 9
- 239000005457 ice water Substances 0.000 claims description 8
- 235000003270 potassium fluoride Nutrition 0.000 claims description 8
- 239000011698 potassium fluoride Substances 0.000 claims description 8
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- 229910000990 Ni alloy Inorganic materials 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 238000010348 incorporation Methods 0.000 claims description 2
- PCLURTMBFDTLSK-UHFFFAOYSA-N nickel platinum Chemical compound [Ni].[Pt] PCLURTMBFDTLSK-UHFFFAOYSA-N 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 13
- 239000013078 crystal Substances 0.000 abstract description 9
- 230000015572 biosynthetic process Effects 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 55
- 238000004458 analytical method Methods 0.000 description 18
- 238000001069 Raman spectroscopy Methods 0.000 description 13
- 238000002360 preparation method Methods 0.000 description 13
- 238000005303 weighing Methods 0.000 description 13
- 238000002347 injection Methods 0.000 description 12
- 239000007924 injection Substances 0.000 description 12
- 238000012790 confirmation Methods 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 8
- 238000003556 assay Methods 0.000 description 6
- 238000002386 leaching Methods 0.000 description 6
- 239000013589 supplement Substances 0.000 description 6
- 239000002131 composite material Substances 0.000 description 5
- 230000007062 hydrolysis Effects 0.000 description 5
- 238000006460 hydrolysis reaction Methods 0.000 description 5
- 238000002203 pretreatment Methods 0.000 description 5
- 239000003643 water by type Substances 0.000 description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 239000003990 capacitor Substances 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 229910019804 NbCl5 Inorganic materials 0.000 description 3
- 238000007605 air drying Methods 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000009423 ventilation Methods 0.000 description 3
- 229910019648 Nb(OH)3 Inorganic materials 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000002127 nanobelt Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- YHBDIEWMOMLKOO-UHFFFAOYSA-I pentachloroniobium Chemical compound Cl[Nb](Cl)(Cl)(Cl)Cl YHBDIEWMOMLKOO-UHFFFAOYSA-I 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000186216 Corynebacterium Species 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- TTXOCPWHRPZIJA-UHFFFAOYSA-N [F].[Nb] Chemical compound [F].[Nb] TTXOCPWHRPZIJA-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- JUWSSMXCCAMYGX-UHFFFAOYSA-N gold platinum Chemical compound [Pt].[Au] JUWSSMXCCAMYGX-UHFFFAOYSA-N 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 229910000484 niobium oxide Inorganic materials 0.000 description 1
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000013433 optimization analysis Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002887 superconductor Substances 0.000 description 1
- 230000010415 tropism Effects 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G33/00—Compounds of niobium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-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
- C01P2004/10—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
-
- 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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Crystallography & Structural Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
It prepares to have the invention discloses a kind of use single agents autoreaction and aligns Nb2O5The method of nanometer rods, includes the following steps：(1) it chooses potassium niobate fluoride powder to be dissolved in deionized water, potassium niobate fluoride weak solution is placed in the golden pipe of your pretreated gold, sealing；(2) noble metal pipe is placed in hydrothermal reaction kettle and sealed, it is 200~500 DEG C to adjust hydro-thermal reaction temperature in the kettle, and inert gas or deionized water is used to adjust in hydrothermal reaction kettle pressure as 50~200MPa, reaction 12~for 24 hours is hydrolyzed, reaction kettle is cooled to room temperature after reaction；(3) hydrothermal reaction kettle is opened, take out the noble metal pipe after reaction and is opened, recycles residual solution, collects sample, acquisition aligns Nb2O5Nanometer rods.This method is using single agents as synthesis material, and raw material is simple, is easy to get, and of low cost, energy consumption is small, the Nb prepared2O5Nanometer rods crystal form is intact, and directionality is notable.
Description
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of single agents autoreaction is prepared to have and be aligned
Nb2O5The method of nanometer rods.
Background technology
Nb2O5As a kind of typical n-type semiconductor, there is acid-alkali-corrosive-resisting property, excellent optical property and steady
Fixed superior electrochemical properties make it be passed in capacitor, light-guide material, superconductor, photoelectrocatalysis, solar cell, biology
Sensor and lithium ion battery etc. all have a wide range of applications potentiality, especially in the electronics material such as capacitor, lithium ion battery
There is huge potential application in terms of material.
Early in 1981, Reichman etc. was for the first time by Nb2O5As original electrode material of lithium battery, Koshiba etc. 1994
Year has studied Nb under various configuration2O5Electrochemical properties, but that use is all Nb for these researchs2O5Particle.Until 2008,
Report Wei etc. utilizes niobium powder and niobium source for the first time, by the solvent structure Nb for being up to 14 days2O5Nanobelt simultaneously has as electrode
Good effect.One-dimensional Nb2O5Nano material (nanometer rods, nanotube, nanobelt, nanofiber) just start electrode for capacitors,
Lithium ion battery etc. extensive utilization.
Related Nb at present2O5The report of nanometer rods synthesis is relatively fewer, such as 2013, yellow to wait suddenly with NbCl5For single niobium
Source under the conditions of no dispersant, prepares that pattern is uniform, the smaller one-dimensional Nb of size by mono- step solvent-thermal methods of 72h2O5Nanometer rods,
2015, the quick beautiful grade of fourth was with columbium pentachloride (NbCl5) and graphene oxide (GO) be raw material, synthesized using uv irradiation method
NbCl5Nanometer rods.
Current various Nb2O5The synthetic method of nanometer rods is generally relatively complicated, has or the spies such as high cost or high energy consumption
Point, and the Nb synthesized2O5Nanometer rods directionality is poor.This constrains Nb to a certain extent2O5Nanometer rods are in industrial production
With and promote.
Invention content
It prepares to have the purpose of the present invention is to provide a kind of single agents autoreaction and aligns Nb2O5The side of nanometer rods
Method, this method is using single agents as synthesis material, and raw material is simple, is easy to get, and of low cost, energy consumption is small, prepares
Nb2O5Nanometer rods crystal form is intact, and directionality is notable.
The above-mentioned purpose of the present invention is achieved by the following technical solution：A kind of single agents autoreaction preparation has
Align Nb2O5The method of nanometer rods, includes the following steps：
(1) it is soluble in water to choose potassium niobate fluoride powder, obtains potassium niobate fluoride weak solution, potassium niobate fluoride weak solution is placed in pre-
In processed noble metal pipe, then by the noble metal seal of tube；
(2) the noble metal pipe being sealed is placed in hydrothermal reaction kettle, then seals hydrothermal reaction kettle, it is anti-to adjust hydro-thermal
Temperature in the kettle is answered as 200~500 DEG C, and use in inert gas or deionized water adjusting hydrothermal reaction kettle pressure for 50~
200MPa is hydrolyzed reaction 12~for 24 hours, hydrothermal reaction kettle is cooled to room temperature after reaction；
(3) hydrothermal reaction kettle is opened, take out the noble metal pipe after reaction and is opened, recycles residual solution, collects sample, institute
Sample it is washed, it is dry after obtain and align Nb2O5Nanometer rods.
It prepares to have in above-mentioned use single agents autoreaction and aligns Nb2O5In the method for nanometer rods：
Potassium niobate fluoride (K described in step (1)2NbF7) weak solution a concentration of 0.005~0.02mol/L, the fluorine niobium
The volume of sour potassium weak solution accounts for the 40%~70% of noble metal pipe total volume.
Potassium niobate fluoride (K wherein described in step (1)2NbF7) powder Optimization Analysis purity grade, impurity is avoided to experiment
Interference.
Water is preferably deionized water or distilled water in step (1).
The pretreatment of noble metal pipe described in step (1) is：Noble metal pipe is chosen, through including truncation, acid boils, washs and quenches
Fire processing, so that it is guaranteed that influencing to test, and ensure the complete seal of noble metal pipe without other impurities in noble metal pipe.
Noble metal described in step (1) preferably refers to silver, gold, platinum gold, silver target, gold-palladium or platinum-nickel alloys.
When in step (1) by noble metal pipe complete seal, potassium niobate fluoride weak solution is first placed in sealing in noble metal pipe, so
Temperature is adjusted afterwards weighs noble metal pipe again, really for 100 DEG C~120 DEG C drying more than 2h, more preferably 110 DEG C drying more than 2h
Quality error is less than 0.001g before and after guarantor.So as to ensure its validity for being fully sealed, testing.
Reaction time in step (2) does not include heating and cools down the consumed time, is anti-under assigned temperature and pressure
Between seasonable.
Inert gas described in step (2) is argon gas or helium.
Fast cooling is carried out to reaction kettle using ice water during cooling in step (2) or constant pressure cools down.
Noble metal pipe need to carry out clean, dry, weighing to ensure the validity of experiment progress after being reacted in step (3).
Residual solution described in step (3) includes potassium niobate fluoride, hydrofluoric acid and potassium fluoride, recycling residual solution include to
Incorporation oxidation niobium powder, hydrofluoric acid and potassium fluoride are continued to synthesize potassium niobate fluoride, made as initial reaction solution in residual solution
With so as to eliminate hydrofluoric acid pollution to a certain extent.
When sample is collected in step (3), residual solution is first taken out, it will be in noble metal pipe with deionized water and absolute ethyl alcohol
Wall respectively washing 2~3 times, ensure the cleaning of sample, then collect the sample being attached on noble metal inside pipe wall, have to obtain the final product after dry
Align Nb2O5Nanometer rods.Drying can be preserved using air-dried or drying basin.
The present invention, which prepares to have using single agents autoreaction, aligns Nb2O5The core of the method for nanometer rods is profit
Nb is generated by the hydrolysis of itself under the conditions of specific temperature and pressure with potassium niobate fluoride single agents2O5Nanometer rods, institute
Sole agent is potassium niobate fluoride solution, and under hydrothermal conditions, with water successively following hydrolysis occurs for potassium niobate fluoride：
K2NbF7+H2O=K2Nb(OH)F6+HF
K2Nb(OH)F6+H2O=K2Nb(OH)2F5+HF
K2Nb(OH)2F5+H2O=K2Nb(OH)3F4+HF
K2Nb(OH)3F4+H2O=K2Nb(OH)4F3+HF
K2Nb(OH)4F3+H2O=Nb (OH)5+2KF+HF
2Nb(OH)5=Nb2O5↓+5H2O
Hydrolysis, which occurs, for potassium niobate fluoride can generate Nb2O5And potassium, hydrogen, fluorine ion, the fluorine ion in product can reduce Nb2O5
(001) the surface energy in face promotes the growth in (001) face, final so that synthesis aligns Nb2O5Nanometer rods, so as to avoid biography
The reagents such as hydrofluoric acid are additionally added in system technique.
Compared with prior art, the invention has the advantages that：
(1) method of the invention aligns Nb by the synthesis of single agents autoreaction2O5Nanometer rods avoid traditional work
During skill the proportioning of a variety of predecessors and pattern controlling agent weigh and priority processing step, therefore this method it is simple for process,
Easily operated control, advantage of lower cost；
(2) the method for the present invention using potassium niobate fluoride solution as single agents, by potassium niobate fluoride under hydrothermal conditions oneself
The hydrolysis generation of body aligns Nb2O5Nanometer rods, while the hydrogen ion and fluorine ion that generate add instead of in traditional handicraft
The hydrofluoric acid entered aligns Nb so as to fulfill the generation of single agents autoreaction2O5Nanometer rods；
(3) the method for the present invention using high-purity noble metal pipe make housing can ensure reactant not with other substance reactions,
The leakproofness and validity of reaction process, at low cost, energy consumption is small；
(4) the method for the present invention aligns Nb by the incomplete hydrolysis synthesis of potassium niobate fluoride itself2O5Nanometer rods,
Solution is recycled mainly comprising potassium niobate fluoride, hydrofluoric acid and potassium fluoride, and recycling solution such as mixes niobium oxide thereto by processing
Powder can continue hydrofluoric acid and potassium fluoride to synthesize potassium niobate fluoride, and the recycling solution obtained can continue on for the first of the present invention
Beginning raw material, on the one hand effectively can recycle and reduce cost, on the other hand can eliminate hydrofluoric acid pollution, maintain process safety, focus on
Environmental protection；
(5) Nb prepared using the method for the present invention2O5Nanorod length be hundreds of nanometers to tens microns, a diameter of more than ten
Nanometer is to tens nanometers or even to hundreds of nanometers, relative to existing synthetic method, the Nb of this method acquisition2O5Nanometer rods are determined
Tropism is more preferable, and crystal form is more complete, thus has huge potential application valency in terms of the electronic materials such as capacitor, lithium ion battery
Value.
Description of the drawings
Fig. 1 aligns Nb for what is prepared in 1-6 of the embodiment of the present invention2O5The LR laser raman collection of illustrative plates of nanometer rods；
Fig. 2 aligns Nb for what is prepared in the embodiment of the present invention 12O5The stereoscan photograph of nanometer rods；
Fig. 3 aligns Nb for what is prepared in the embodiment of the present invention 22O5The stereoscan photograph of nanometer rods；
Fig. 4 aligns Nb for what is prepared in the embodiment of the present invention 32O5The stereoscan photograph of nanometer rods；
Fig. 5 aligns Nb for what is prepared in the embodiment of the present invention 42O5The stereoscan photograph of nanometer rods；
Fig. 6 is the single Nb prepared in the embodiment of the present invention 52O5The stereoscan photograph of nanometer rods；
Fig. 7 aligns Nb for what is prepared in the embodiment of the present invention 62O5The stereoscan photograph of nanometer rods, (a) are
Orient Nb2O5Nanometer rods photo, (b) is can radial Nb2O5Nanometer rods photo.
Specific embodiment
With reference to embodiment and attached drawing, the present invention is further illustrated, but the scope of protection of present invention is for example anti-
Answer device and reaction temperature, the volume of reaction time and reaction liquid is not limited to embodiment and is lifted.
Embodiment 1
It is provided in this embodiment to align Nb2O5The preparation method of nanometer rods, includes the following steps：
(1) the high-purity gold pipe of a diameter of 3~5mm is truncated into 4cm, is placed in that be mounted with 0.01mol/L dust technologies molten
In the beaker of liquid, beaker is placed in 80 DEG C of heating plates and carries out boiling two hours；It washs, dry and one through deionized water again
End shifts to an earlier date the processing early periods such as sealing, it is ensured that free from admixture and crack in golden pipe；
(2) by the potassium niobate fluoride (K of 0.76g purity assays2NbF7, commercial product, similarly hereinafter) and powder is dissolved in 250mL deionizations
In water, a concentration of 0.01mol/L K are made in fully dissolving2NbF7The reaction solution of preparation is taken about 0.2mL to put into gold pipe by solution
Interior, compactedness control is 40%~70% or so, and carries out sealing, and weighing record is carried out after sealing, then solution sample will be housed
The golden pipe of product is put into 110 DEG C of more than drying box 2h, after weighed again, it is ensured that it is front and rear weighing quality error be less than 0.001g,
Illustrate that golden composite pipe tightness is intact；
(3) it will confirm that leakproofness is intact and the golden pipe of solution example is housed and put nickel-base alloy hydrothermal reaction kettle into, tighten anti-
After answering kettle, check the leakproofness of reaction kettle, confirm it is errorless after pumped by gas boosting argon gas injected into kettle to pressure 50MPa,
It as initial pressure, closes shut-off valve and stops gas injection, reaction kettle is heated by heating furnace, setting reaction temperature is 200
℃；
(4) temperature is risen to after 200 DEG C, shut-off valve in opening steps (3), continues supplement injection argon gas to pressure 100MPa
And keep stablizing and reaction 12h is carried out under Temperature-pressure Conditions, pouring reaction kettle in leaching step (3) using ice water after the completion of reaction carries out quickly
Cooling or constant pressure are cooled to room temperature；
(5) reaction kettle in step (4) is opened, the golden pipe in reaction kettle is taken out, is clean, dries and weighs, it is ensured that is anti-
The leakproofness and validity of process are answered, golden pipe is broken after confirmation is errorless, recycles its residual solution, washed using deionized water, alcohol
It washs golden inside pipe wall each 2~3 times, makes to be attached to the Nb of golden inside pipe wall2O5Sample is clean, then deposit sample air-dried with natural wind or
Person can obtain aligning Nb after drying ware drying2O5Nanometer rods；
(6) by the Nb of acquisition2O5Sample carries out Raman analysis and morphology analysis, and Fig. 1 (a) is for LR laser raman analysis shows that institute
The nanometer rods of acquisition are Nb2O5Nanometer rods, the Nb of Fig. 2 stereoscan photographs display synthesis2O5Nanometer rods are into oriented structure, face
Camera lens is (001) face, and rodlike crystal form is complete；
(7) residual solution is mainly potassium niobate fluoride, hydrofluoric acid and potassium fluoride, this solution is handled, and is such as mixed thereto
Enter niobium powder, hydrofluoric acid and potassium fluoride can be continued to synthesize potassium niobate fluoride, can still be re-used as above-mentioned initial reaction solution.
Embodiment 2
It is provided in this embodiment to align Nb2O5The preparation method of nanometer rods, includes the following steps：
(1) pre-treatment of platinum pipe is the same as embodiment 1；
(2) by the potassium niobate fluoride (K of 0.38g purity assays2NbF7) powder is dissolved in 250mL deionized waters, abundant dissolving system
Obtain 0.005mol/L K2NbF7The reaction solution of preparation is taken about 0.2mL to put into platinum pipe by solution, and compactedness control is 40%
~70% or so, and sealing is carried out, weighing record is carried out after sealing, the platinum pipe equipped with solution example is then put into 110 DEG C
More than drying box 2h, after weighed again, it is ensured that it is front and rear weighing quality error be less than 0.001g, illustrate that golden composite pipe tightness is complete
It is good；
(3) it will confirm that leakproofness is intact and the platinum pipe of solution example is housed and put high-temperature high-pressure reaction kettle into, tighten reaction
After kettle, check the leakproofness of reaction kettle, deionized water is injected to pressure into kettle by liquid booster pump after confirmation is errorless
60MPa as initial pressure, closes shut-off valve and stops gas injection, reaction kettle is heated by heating furnace, set reaction temperature
It is 300 DEG C；
(4) temperature is risen to after 300 DEG C, shut-off valve in opening steps (3), continues supplement injection deionized water to pressure
200MPa simultaneously keeps stablizing reaction 12h is carried out under Temperature-pressure Conditions, after the completion of reaction using ice water pour in leaching step (3) reaction kettle into
Row fast cooling or constant pressure are cooled to room temperature；
(5) reaction kettle in step (4) is opened, the platinum pipe in reaction kettle is taken out, is clean, dries and weighs, it is ensured that
The leakproofness and validity of reaction process break platinum pipe after confirmation is errorless, recycle its residual solution, use deionized water, wine
Fine purifiation washs platinum inside pipe wall each 2~3 times, makes to be attached to the Nb of platinum inside pipe wall2O5Sample is clean, then by deposit sample nature
Wind can obtain aligning Nb after air-drying or drying ware drying2O5Nanometer rods；
(6) by the Nb of acquisition2O5Sample carries out Raman analysis and morphology analysis, and Fig. 1 (b) is for LR laser raman analysis shows that institute
The nanometer rods of acquisition are Nb2O5Nanometer rods, the Nb of Fig. 3 stereoscan photographs display synthesis2O5Nanometer rods are into oriented structure, crystal form
Completely, part Nb2O5Sample is in corynebacterium；
(7) recycling of residual solution is the same as embodiment 1.
Embodiment 3
It is provided in this embodiment to align Nb2O5The preparation method of nanometer rods, includes the following steps：
(1) pre-treatment of gold-palladium pipe is the same as embodiment 1；
(2) by the potassium niobate fluoride (K of 0.76g purity assays2NbF7) powder is dissolved in 250mL deionized waters, abundant dissolving system
Obtain 0.01mol/L K2NbF7The reaction solution of preparation is taken about 0.2mL to put into gold-palladium pipe by solution, and compactedness control is 40%
~70% or so, and sealing is carried out, weighing record is carried out after sealing, the gold-palladium pipe equipped with solution example is then put into 110 DEG C
More than drying box 2h, after weighed again, it is ensured that it is front and rear weighing quality error be less than 0.001g, illustrate that gold-palladium composite pipe tightness is complete
It is good；
(3) it will confirm that leakproofness is intact and the gold-palladium pipe of solution example is housed and put high-temperature high-pressure reaction kettle into, tighten reaction
After kettle, check the leakproofness of reaction kettle, confirm it is errorless after argon gas is injected into kettle by ventilation pipe to pressure 60MPa, as
Initial pressure closes shut-off valve and stops gas injection, reaction kettle is heated by heating furnace, and setting reaction temperature is 400 DEG C；
(4) temperature is risen to after 400 DEG C, shut-off valve in opening steps (3), continues supplement injection argon gas to pressure 100MPa
And keep stablizing and be reacted under Temperature-pressure Conditions for 24 hours, pouring reaction kettle in leaching step (3) using ice water after the completion of reaction carries out quickly
Cooling or constant pressure are cooled to room temperature；
(5) reaction kettle in step (4) is opened, the gold-palladium pipe in reaction kettle is taken out, is clean, dries and weighs, it is ensured that
The leakproofness and validity of reaction process break gold-palladium pipe after confirmation is errorless, recycle its residual solution, use deionized water, wine
Fine purifiation washs golden inside pipe wall each 2~3 times, makes to be attached to the Nb of gold-palladium inside pipe wall2O5Sample is clean, then by deposit sample natural wind
It can obtain aligning Nb after air-drying or drying ware drying2O5Nanometer rods；
(6) by the Nb of acquisition2O5Sample carries out Raman analysis and morphology analysis, and Fig. 1 (c) is for LR laser raman analysis shows that institute
The nanometer rods of acquisition are Nb2O5Nanometer rods, the Nb of Fig. 4 stereoscan photographs display synthesis2O5Nanometer rods oriented structure is apparent, brilliant
Type is complete；
(7) recycling of residual solution is the same as embodiment 1.
Embodiment 4
It is provided in this embodiment to align Nb2O5The preparation method of nanometer rods, includes the following steps：
(1) pre-treatment of silver-colored palladium tube is the same as embodiment 1；
(2) by the potassium niobate fluoride (K of 0.76g purity assays2NbF7) powder is dissolved in 250mL deionized waters, abundant dissolving system
Obtain 0.01mol/L K2NbF7The reaction solution of preparation is taken about 0.2mL to put into silver-colored palladium tube by solution, and compactedness control is 40%
~70% or so, and sealing is carried out, weighing record is carried out after sealing, the silver-colored palladium tube equipped with solution example is then put into 110 DEG C
More than drying box 2h, after weighed again, it is ensured that it is front and rear weighing quality error be less than 0.001g, illustrate that silver-colored palladium tube leakproofness is complete
It is good；
(3) it will confirm that leakproofness is intact and the silver-colored palladium tube of solution example is housed and put high-temperature high-pressure reaction kettle into, tighten reaction
After kettle, check the leakproofness of reaction kettle, deionized water is injected to pressure into kettle by liquid booster pump after confirmation is errorless
50MPa as initial pressure, closes shut-off valve and stops gas injection, reaction kettle is heated by heating furnace, set reaction temperature
It is 500 DEG C；
(4) temperature is risen to after 500 DEG C, shut-off valve in opening steps (3), continues supplement injection deionized water to pressure
200MPa simultaneously keeps stablizing reaction 12h is carried out under Temperature-pressure Conditions, after the completion of reaction using ice water pour in leaching step (3) reaction kettle into
Row fast cooling or constant pressure are cooled to room temperature；
(5) reaction kettle in step (4) is opened, the silver-colored palladium tube in reaction kettle is taken out, is clean, dries and weighs, it is ensured that
The leakproofness and validity of reaction process break silver-colored palladium tube after confirmation is errorless, recycle its residual solution, use deionized water, wine
Fine purifiation washs golden inside pipe wall each 2~3 times, makes to be attached to the Nb of silver-colored palladium tube inner wall2O5Sample is clean, then by deposit sample natural wind
It can obtain aligning Nb after air-drying or drying ware drying2O5Nanometer rods；
(6) by the Nb of acquisition2O5Sample carries out Raman analysis and morphology analysis, and Fig. 1 (d) is for LR laser raman analysis shows that institute
The nanometer rods of acquisition are Nb2O5Nanometer rods, the Nb of Fig. 5 stereoscan photographs display synthesis2O5Nanometer rods are into oriented structure, crystal form
Completely；
(7) recycling of residual solution is the same as embodiment 1.
Embodiment 5
It is provided in this embodiment to align Nb2O5The preparation method of nanometer rods, includes the following steps：
(1) pre-treatment of silver-colored pipe is the same as embodiment 1；
(2) by the potassium niobate fluoride (K of 0.76g purity assays2NbF7) powder is dissolved in 250mL deionized waters, abundant dissolving system
Obtain 0.01mol/L K2NbF7The reaction solution of preparation is taken about 0.2mL to put into silver-colored pipe by solution, compactedness control for 40%~
70% or so, and sealing is carried out, weighing record is carried out after sealing, the silver-colored pipe equipped with solution example is then put into 110 DEG C of drying
More than case 2h, after weighed again, it is ensured that it is front and rear weighing quality error be less than 0.001g, illustrate that silver-colored composite pipe tightness is intact；
(3) will confirm that leakproofness is intact and silver-colored pipe equipped with solution example puts high-temperature high-pressure reaction kettle into, and inject go from
Sub- water after tightening reaction kettle, checks the leakproofness of reaction kettle, is injected after confirmation is errorless by ventilation pipe into kettle as medium
Argon gas as initial pressure, closes shut-off valve and stops gas injection, reaction kettle is heated by heating furnace to pressure 60MPa, if
It is 200 DEG C to put reaction temperature；
(4) temperature is risen to after 200 DEG C, shut-off valve in opening steps (3), continues supplement injection argon gas to pressure 100MPa
And keep stablizing and reaction 23h is carried out under Temperature-pressure Conditions, pouring reaction kettle in leaching step (3) using ice water after the completion of reaction carries out quickly
Cooling or constant pressure are cooled to room temperature；
(5) reaction kettle in step (4) is opened, the silver-colored pipe in reaction kettle is taken out, is clean, dries and weighs, it is ensured that is anti-
The leakproofness and validity of process are answered, silver-colored pipe is broken after confirmation is errorless, recycles its residual solution, washed using deionized water, alcohol
It washs golden inside pipe wall each 2~3 times, makes to be attached to the Nb of silver-colored inside pipe wall2O5Sample is clean, then deposit sample air-dried with natural wind or
Person can obtain aligning Nb after drying ware drying2O5Nanometer rods；
(6) by the Nb of acquisition2O5Sample carries out Raman analysis and morphology analysis, and Fig. 1 (e) is for LR laser raman analysis shows that institute
The nanometer rods of acquisition are Nb2O5Nanometer rods, the Nb of Fig. 6 stereoscan photographs display synthesis2O5Nanometer rods, crystal form is more complete, length
It is 150~250 nanometers；
(7) recycling of residual solution is the same as embodiment 1.
Embodiment 6
It is provided in this embodiment to align Nb2O5The preparation method of nanometer rods, includes the following steps：
(1) pre-treatment of golden pipe is the same as embodiment 1；
(2) by the potassium niobate fluoride (K of 1.52g purity assays2NbF7) powder is dissolved in 250mL deionized waters, abundant dissolving system
Obtain 0.02mol/L K2NbF7The reaction solution of preparation is taken about 0.2mL to put into golden pipe by solution, compactedness control for 40%~
70% or so, and sealing is carried out, weighing record is carried out after sealing, the golden pipe equipped with solution example is then put into 110 DEG C of drying
More than case 2h, after weighed again, it is ensured that it is front and rear weighing quality error be less than 0.001g, illustrate that golden composite pipe tightness is intact；
(3) it will confirm that leakproofness is intact and the golden pipe of solution example is housed and put high-temperature high-pressure reaction kettle into, tighten reaction kettle
Afterwards, check the leakproofness of reaction kettle, confirm it is errorless after inject into kettle argon gas by ventilation pipe to pressure 60MPa, as
Beginning pressure closes shut-off valve and stops gas injection, reaction kettle is heated by heating furnace, and setting reaction temperature is 200 DEG C；
(4) temperature is risen to after 200 DEG C, shut-off valve in opening steps (3), continues supplement injection argon gas to pressure 100MPa
And keep stablizing and reaction 12h is carried out under Temperature-pressure Conditions, pouring reaction kettle in leaching step (3) using ice water after the completion of reaction carries out quickly
Cooling or constant pressure are cooled to room temperature；
(5) reaction kettle in step (4) is opened, the golden pipe in reaction kettle is taken out, is clean, dries and weighs, it is ensured that is anti-
The leakproofness and validity of process are answered, golden pipe is broken after confirmation is errorless, recycles its residual solution, washed using deionized water, alcohol
It washs golden inside pipe wall each 2~3 times, makes to be attached to the Nb of golden inside pipe wall2O5Sample is clean, then deposit sample air-dried with natural wind or
Person can obtain aligning Nb after drying ware drying2O5Nanometer rods；
(6) by the Nb of acquisition2O5Sample carries out Raman analysis and morphology analysis, and Fig. 1 (f) is for LR laser raman analysis shows that institute
The nanometer rods of acquisition are Nb2O5Nanometer rods, the orientation Nb of figure (a) stereoscan photograph display synthesis in Fig. 72O5Nanometer rods, crystal form
Completely, the Nb of figure (b) display portion synthesis2O5Nanometer rods are alternatively radial, and crystal form is complete；
(7) recycling of residual solution is the same as embodiment 1.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included in protection scope of the present invention.
Claims (8)
1. a kind of use single agents autoreaction, which prepares to have, aligns Nb2O5The method of nanometer rods, it is characterized in that including following
Step：
(1) it is soluble in water to choose potassium niobate fluoride powder, obtains potassium niobate fluoride weak solution, potassium niobate fluoride weak solution is placed in pretreatment
In the noble metal pipe crossed, then by the noble metal seal of tube；
(2) the noble metal pipe being sealed is placed in hydrothermal reaction kettle, then seals hydrothermal reaction kettle, adjust hydrothermal reaction kettle
Interior temperature be 200~500 DEG C, and use inert gas or deionized water adjusting hydrothermal reaction kettle in pressure for 50~200MPa,
Reaction 12~for 24 hours is hydrolyzed, hydrothermal reaction kettle is cooled to room temperature after reaction；
(3) hydrothermal reaction kettle is opened, take out the noble metal pipe after reaction and is opened, recycles residual solution, collects sample, gained sample
Product are washed, i.e. acquisition aligns Nb after drying2O5Nanometer rods.
2. use single agents autoreaction according to claim 1, which prepares to have, aligns Nb2O5The method of nanometer rods,
It is characterized in that：A concentration of 0.005~0.02mol/L of potassium niobate fluoride weak solution described in step (1), the potassium niobate fluoride are dilute
The volume of solution accounts for the 40%~70% of noble metal pipe total volume.
3. use single agents autoreaction according to claim 1, which prepares to have, aligns Nb2O5The method of nanometer rods,
It is characterized in that the pretreatment of noble metal pipe described in step (1) is：Noble metal pipe is chosen, through including truncation, acid is boiled, washs and done
Dry processing, wherein the noble metal includes gold, silver, platinum, gold-palladium, silver-colored palladium or platinum-nickel alloys.
4. use single agents autoreaction according to claim 1, which prepares to have, aligns Nb2O5The method of nanometer rods,
It is characterized in that：When in step (1) by the noble metal seal of tube, potassium niobate fluoride weak solution is first placed in sealing in noble metal pipe, then
Temperature is adjusted as 100~120 DEG C of drying more than 2h, weighs noble metal pipe again, it is ensured that front and rear quality error is less than 0.001g.
5. use single agents autoreaction according to claim 1, which prepares to have, aligns Nb2O5The method of nanometer rods,
It is characterized in that：Inert gas described in step (2) is argon gas or helium.
6. use single agents autoreaction according to claim 1, which prepares to have, aligns Nb2O5The method of nanometer rods,
It is characterized in that：Fast cooling is carried out to reaction kettle using ice water during cooling in step (2) or constant pressure cools down.
7. use single agents autoreaction according to claim 1, which prepares to have, aligns Nb2O5The method of nanometer rods,
It is characterized in that：Residual solution described in step (3) includes potassium niobate fluoride, hydrofluoric acid and potassium fluoride, and recycling residual solution includes
Into residual solution, incorporation oxidation niobium powder, hydrofluoric acid and potassium fluoride is continued to synthesize potassium niobate fluoride, as initial reaction solution
It uses.
8. use single agents autoreaction according to claim 1, which prepares to have, aligns Nb2O5The method of nanometer rods,
It is characterized in that：When sample is collected in step (3), residual solution is first taken out, with deionized water and absolute ethyl alcohol by noble metal pipe
Then inner wall respectively washing 2~3 times collect the sample being attached on noble metal inside pipe wall, have to obtain the final product after dry and align
Nb2O5Nanometer rods.
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| CN110217835A (en) * | 2019-07-09 | 2019-09-10 | 中国科学院广州地球化学研究所 | A kind of PtO2The preparation method of tapered nano-particle material |
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| CN110203968A (en) * | 2019-06-13 | 2019-09-06 | 中国科学院广州地球化学研究所 | A kind of high (001) face flaky zirconia and preparation method thereof |
| CN110217818A (en) * | 2019-06-13 | 2019-09-10 | 中国科学院广州地球化学研究所 | Uniform particle size zirconium dioxide nanosphere and its film and preparation method |
| CN110217835A (en) * | 2019-07-09 | 2019-09-10 | 中国科学院广州地球化学研究所 | A kind of PtO2The preparation method of tapered nano-particle material |
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