CN107739051A - A kind of method of the hot controlledly synthesis niobium pentaoxide micron ball of no templating solvent and micro-flowers - Google Patents
A kind of method of the hot controlledly synthesis niobium pentaoxide micron ball of no templating solvent and micro-flowers Download PDFInfo
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- CN107739051A CN107739051A CN201711200791.2A CN201711200791A CN107739051A CN 107739051 A CN107739051 A CN 107739051A CN 201711200791 A CN201711200791 A CN 201711200791A CN 107739051 A CN107739051 A CN 107739051A
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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
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- 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
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- 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
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- 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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- 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 belongs to technical field of inorganic nanometer material, and in particular to the method for a kind of hot controlledly synthesis niobium pentaoxide micron ball of no templating solvent and micro-flowers.Comprise the concrete steps that：The inorganic matter ion salt and precipitating reagent of a certain amount of niobium are mixed by a certain percentage first, are dissolved separately in two kinds of different organic solvents；Then ultrasound 15 30 minutes, solid powder is set to be completely dissolved and be well mixed, finally, above-mentioned two parts of solution is transferred in the reactor of polytetrafluoroethylsubstrate substrate respectively, seals, is placed in baking oven, the temperature for controlling baking oven is 180 200 DEG C, react 8 12 hours, after reaction terminates, product is cooled to room temperature；To precipitated product centrifuge, collect solid, with deionized water and absolute ethyl alcohol wash for several times, be dried in vacuo, produce niobium pentaoxide micron ball and micron floral material.
Description
Technical field
The invention belongs to technical field of inorganic nanometer material, and in particular to one kind aoxidizes without the hot controlledly synthesis five of templating solvent
The method of two niobium micron balls and micro-flowers.
Background technology
Niobium pentaoxide is important n-type semiconductor material with wide forbidden band, and energy gap is 3.4 eV, Yin Qite at room temperature
Different layer structure is widely studied for energy storage material field.Niobium pentaoxide is that ion occurs for body phase as energy storage material
Intercalation, ionic radius size match with niobium pentaoxide interlamellar spacing, and can effectively weaken should caused by ion insertion
Power, so, the intercalation/deintercalation of ion will not cause the structural change of niobium pentoxide nano material in itself, be used as energy storage material
When can greatly increase the service life of material.Meanwhile the niobium pentoxide nano material of body phase ion insertion type energy storage is different
Iron, cobalt, nickel, the manganese-base oxide/hydroxide form energy storage mode of redox reaction, body phase energy storage activity material occurs in surface
Expect that utilization rate is high, it is cost-effective；Surface occurs the energy storage of redox reaction type and only carried out on surface, causes active material great
Waste, also, surface generation redox reaction can cause caving in for this body structure of material, so that electrode material uses the longevity
Life substantially reduces.Niobium pentaoxide can be widely used in traffic, space flight, military project, power network, household electrical appliance as energy storage material
Deng energy storage device；Niobium pentaoxide greater band gap, for photocatalysis field, niobium pentaoxide and carbonitride are answered in research at present
Share in Photocatalyzed Hydrogen Production/oxygen.
The synthetic method of metal oxide has much, including hydrothermal/solvent thermal synthesis method, liquid phase self assembly, anodic oxidation
Method, chemical deposition etc..Wherein, hydrothermal/solvent thermal synthesis method is because its is simple to operation, it is not necessary to which special experimental facilities is by section
Grind the favor of worker.The synthesis of this research object niobium pentaoxide in document report more uses hydrothermal/solvent thermal synthesis side
Method, the niobium pentoxide nano stick and micron ball prepared are in the majority, also have using other methods such as oxidizing process to prepare not similar shape
The niobium pentaoxide of looks, such synthetic method need special experimental facilities, complex synthetic route, and experimental drug is often costly.
The content of the invention
The problem of existing for prior art, simple solvent thermal reaction is only used only in this research, by using different
Precipitating reagent, change reaction medium polarity etc. can regulate and control out the niobium pentoxide nano material with different-shape.This experiment is closed
It is simple into method, it is green safe, it is not necessary to special experimental facilities, to test that used drug price is cheap, is easy to get, have very big
Application value.
The purpose of the present invention aims to provide a kind of simple reliably without the hot controlledly synthesis niobium pentaoxide micron of templating solvent
The method of ball and micron floral material.
To achieve the above object, the technical solution adopted by the present invention is the powder by a certain amount of columbium pentachloride and sodium carbonate
It is added to absolute ethyl alcohol；Ethylene glycol；Ultrasound makes solid powder fully dissolve and be well mixed；Then, it is transferred to polytetrafluoroethylene (PTFE)
In the reactor of substrate, after solvent thermal reaction, treat that it is cooled to room temperature, product is centrifuged, collected；Deionization is used respectively
Water and absolute ethyl alcohol wash for several times to product, re-dry, obtain target product.
The method of a kind of hot controlledly synthesis niobium pentaoxide micron ball of no templating solvent and micro-flowers, comprises the following steps：
（1）The preparation of niobium pentaoxide precursor solution：
The inorganic matter ion salt and precipitating reagent of niobium are mixed by a certain percentage, then by mixture be dissolved separately in two kinds it is different
In organic solvent, niobium pentaoxide precursor solution is made, it is standby；
（2）The preparation of niobium pentaoxide micron ball and micro-flowers：
By step（1）The niobium pentaoxide precursor solution of middle preparation is poured into beaker, ultrasonic 15-30min, is then transferred into poly-
In the reactor of tetrafluoroethene substrate, it is placed in baking oven and reacts, reaction is cooled to room temperature after terminating, and obtains niobium pentaoxide micron
Ball and micro-flowers, it is pending,
（3）The post processing of niobium pentaoxide micron ball and micro-flowers：
By step（2）The niobium pentaoxide micron ball and micro-flowers of gained centrifuge, and collect, respectively with deionized water and anhydrous
Ethanol cleans for several times, dries 2-5 hours at 60-80 DEG C in vacuum desiccator, produces niobium pentoxide nano material.
Step（1）In, two kinds of solvents are absolute ethyl alcohol, ethylene glycol respectively.
Step（1）In, the inorganic matter ion salt of the niobium of addition and the mol ratio of precipitating reagent are 1:5.
Step（1）In, the inorganic matter ion salt of described niobium is columbium pentachloride or niobium oxalate.
Step（1）In, described precipitating reagent is sodium carbonate or ammonium carbonate.
Step（2）In, described reaction temperature is 180-200 DEG C.
Step（2）In, the described reaction time is 8-12 hours.
Using the inventive method prepare material structure and pattern can be respectively adopted X-ray powder diffraction (XRD) and
ESEM（SEM）, transmission electron microscope (TEM) characterized.
The invention has the advantages that：
1st, the invention provides the method for a kind of hot controlledly synthesis niobium pentaoxide micron ball of no templating solvent and micron floral material,
The niobium pentaoxide micron ball and micro-flowers size prepared using the present invention is smaller, is evenly distributed.
2nd, experiment condition of the present invention is simple, it is not necessary to special experimental facilities；Used solvent is cheap, nontoxic nothing
Evil, meet the friendly requirement of environment green, have and be extremely widely applied prospect.
Brief description of the drawings
Fig. 1 is the X-ray powder diffraction figure (XRD) of niobium pentoxide nano material obtained by 1-2 of the embodiment of the present invention；
Fig. 2 is the scanning electron microscopic picture of the gained niobium pentaoxide micron ball of the embodiment of the present invention 1（SEM）（A）And transmission electron microscope picture
Piece（TEM）（B）；
Fig. 3 is the gained niobium pentaoxide micro-flowers scanning electron microscopic picture of the embodiment of the present invention 2（SEM）.
Embodiment
The present invention is expanded on further below by example, but protection scope of the present invention is not limited to these examples.This
Raw material in invention example is purchased from Shanghai Chinese medicines group, is that analysis is pure.
Example 1：
The powder of 1.5 mmol columbium pentachloride and 7.5 mmol sodium carbonate is added into 30 mL absolute ethyl alcohols, is placed in 100 mL burnings
In cup, being put into ultrasound in Ultrasound Instrument makes it well mixed for 15 minutes, is subsequently poured into the reactor of 50 mL polytetrafluoroethylsubstrate substrates
In, sealing, it is placed in baking oven, the temperature for controlling baking oven is 200 DEG C, is reacted 12 hours, and reaction cools to room temperature with the furnace after terminating,
Precipitated product is centrifuged, wash multiple, 80 DEG C of dryings 3 hours with deionized water and absolute ethyl alcohol, it is micro- to produce niobium pentaoxide
Rice ball.In Fig. 1, there are not other miscellaneous peaks, each diffraction maximum position and relative intensity with JPCDS cards（28-0317）Phase
It coincide, shows the niobium pentaoxide that product is class hexagonal structure.Micron bulb diameter is about 1.2 microns as can be seen from Figure 2.
Example 2：
The powder of 1.5 mmol columbium pentachloride and 7.5 mmol sodium carbonate is added into 30 mL ethylene glycol, is placed in 100 mL beakers
In, being put into ultrasound in Ultrasound Instrument makes it well mixed for 15 minutes, is subsequently poured into the reactor of 50 mL polytetrafluoroethylsubstrate substrates,
Sealing, is placed in baking oven, and the temperature for controlling baking oven is 200 DEG C, is reacted 12 hours, and reaction cools to room temperature with the furnace after terminating, from
Heart precipitation and separation product, washed repeatedly with deionized water and absolute ethyl alcohol, 80 DEG C of dryings 3 hours, produce niobium pentoxide nano
Flower.Nanometer flower diameter is about 3.6 microns as can be seen from Figure 3, is made up of nanometer sheet, and thickness is about 12 nanometers.
Description to examples detailed above is understood that for ease of those skilled in the art and using the present invention.It is ripe
Know the personnel of art technology obviously can easily make various modifications to these examples, and General Principle described herein
It is applied in other examples without by performing creative labour.Therefore, the invention is not restricted to example here, art technology
For personnel according to the announcement of the present invention, the improvement made for the present invention and modification all should be within protection scope of the present invention.
Claims (7)
1. the method for a kind of hot controlledly synthesis niobium pentaoxide micron ball of no templating solvent and micro-flowers, it is characterised in that including
Following steps：
（1）The preparation of niobium pentaoxide precursor solution：
The inorganic matter ion salt and precipitating reagent of niobium are mixed by a certain percentage, then by mixture be dissolved separately in two kinds it is different
In organic solvent, niobium pentaoxide precursor solution is made, it is standby；
（2）The preparation of niobium pentaoxide micron ball and micro-flowers：
By step（1）The niobium pentaoxide precursor solution of middle preparation is poured into beaker, ultrasonic 15-30min, is then transferred into poly-
In the reactor of tetrafluoroethene substrate, it is placed in baking oven and reacts, reaction is cooled to room temperature after terminating, and obtains niobium pentaoxide micron
Ball and micro-flowers, it is pending；
（3）The post processing of niobium pentaoxide micron ball and micro-flowers：
By step（2）The niobium pentaoxide micron ball and micro-flowers of gained centrifuge, and collect, respectively with deionized water and anhydrous
Ethanol cleans for several times, dries 2-5 hours at 60-80 DEG C in vacuum desiccator, produces niobium pentoxide nano material.
2. the side of a kind of hot controlledly synthesis niobium pentaoxide micron ball of no templating solvent according to claim 1 and micro-flowers
Method, it is characterised in that step（1）In, two kinds of solvents are absolute ethyl alcohol, ethylene glycol respectively.
3. the side of a kind of hot controlledly synthesis niobium pentaoxide micron ball of no templating solvent according to claim 1 and micro-flowers
Method, it is characterised in that step（1）In, the inorganic matter ion salt of the niobium of addition and the mol ratio of precipitating reagent are 1:5.
4. the side of a kind of hot controlledly synthesis niobium pentaoxide micron ball of no templating solvent according to claim 1 and micro-flowers
Method, it is characterised in that step（1）In, the inorganic matter ion salt of described niobium is columbium pentachloride or niobium oxalate.
5. the side of a kind of hot controlledly synthesis niobium pentaoxide micron ball of no templating solvent according to claim 1 and micro-flowers
Method, it is characterised in that step（1）In, described precipitating reagent is sodium carbonate or ammonium carbonate.
6. the side of a kind of hot controlledly synthesis niobium pentaoxide micron ball of no templating solvent according to claim 1 and micro-flowers
Method, it is characterised in that step（2）In, described reaction temperature is 180-200 DEG C.
7. the side of a kind of hot controlledly synthesis niobium pentaoxide micron ball of no templating solvent according to claim 1 and micro-flowers
Method, it is characterised in that step（2）In, the described solvent thermal reaction time is 8-12 hours.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109746015A (en) * | 2018-12-14 | 2019-05-14 | 江苏大学 | A kind of high electron hole pair separative efficiency composite photo-catalyst and preparation method thereof |
| CN111334355A (en) * | 2018-12-19 | 2020-06-26 | 中国科学技术大学 | Preparation method of carbon-based fuel and preparation method of niobium pentoxide ultrathin sheet |
| CN111943523A (en) * | 2020-08-24 | 2020-11-17 | 上海第二工业大学 | Niobium pentoxide electrochromic film, hydrothermal synthesis method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105384193A (en) * | 2015-12-09 | 2016-03-09 | 郑州轻工业学院 | Preparation method of niobium (V) pentoxide urchin-like nano sphere and application of nano sphere as photocatalyst |
| CN105958113A (en) * | 2016-06-23 | 2016-09-21 | 南阳师范学院 | Niobium pentoxide mesoporous microsphere electrode material and preparation method therefor |
| 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 |
-
2017
- 2017-11-27 CN CN201711200791.2A patent/CN107739051A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105384193A (en) * | 2015-12-09 | 2016-03-09 | 郑州轻工业学院 | Preparation method of niobium (V) pentoxide urchin-like nano sphere and application of nano sphere as photocatalyst |
| CN105958113A (en) * | 2016-06-23 | 2016-09-21 | 南阳师范学院 | Niobium pentoxide mesoporous microsphere electrode material and preparation method therefor |
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 同济大学普通化学及无机化学教研室: "《普通化学》", 31 July 2004 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109746015A (en) * | 2018-12-14 | 2019-05-14 | 江苏大学 | A kind of high electron hole pair separative efficiency composite photo-catalyst and preparation method thereof |
| CN109746015B (en) * | 2018-12-14 | 2022-02-15 | 江苏大学 | Composite photocatalyst with high electron hole pair separation efficiency and preparation method thereof |
| CN111334355A (en) * | 2018-12-19 | 2020-06-26 | 中国科学技术大学 | Preparation method of carbon-based fuel and preparation method of niobium pentoxide ultrathin sheet |
| CN111334355B (en) * | 2018-12-19 | 2021-07-06 | 中国科学技术大学 | Preparation method of carbon-based fuel and preparation method of niobium pentoxide ultrathin sheet |
| CN111943523A (en) * | 2020-08-24 | 2020-11-17 | 上海第二工业大学 | Niobium pentoxide electrochromic film, hydrothermal synthesis method and application thereof |
| CN111943523B (en) * | 2020-08-24 | 2022-08-09 | 上海第二工业大学 | Niobium pentoxide electrochromic film, hydrothermal synthesis method and application thereof |
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