CN106929876A - The preparation method of metal oxide nano ball - Google Patents
The preparation method of metal oxide nano ball Download PDFInfo
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- CN106929876A CN106929876A CN201710300029.5A CN201710300029A CN106929876A CN 106929876 A CN106929876 A CN 106929876A CN 201710300029 A CN201710300029 A CN 201710300029A CN 106929876 A CN106929876 A CN 106929876A
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- negative electrode
- oxide nano
- metal oxide
- preparation
- nano ball
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
Abstract
The invention provides a kind of preparation method of metal oxide nano ball, including herein below：In an electrolytic cell, anode is Pt pieces, and negative electrode is wire, and electrolyte uses high conductivity salting liquid, and the area ratio that anode and negative electrode immerse electrolyte is anode：Negative electrode=20：1；Using the Iarge Power DC Voltage Regulator of continuously adjustabe, by progressively high voltage, plasma discharge is formed in negative electrode, while forming sediment in the solution, sediment is purified, that is, obtain metal oxide nano ball.The advantage of the invention is that：Participated in without poisonous and harmful chemical reagent, with low cost, simple to operate, material yield is high, expansibility is strong, is had a extensive future in industrial production.
Description
Technical field
Present invention relates particularly to a kind of preparation method of metal oxide nano ball.
Background technology
Nanometer technology is the focus of current mankind front line science, and nano material is due to its small size, high surface energy and big ratio
The features such as surface area so that they show some special natures not available for conventional blocks material, such as small-size effect,
Skin effect, quantum size effect, Dielectric confinement effect and macro quanta tunnel effect etc..Metal oxide nano-material can be answered
For catalyst, fine ceramics, composite, magnetic material, fluorescent material, moisture-sensitive sensor and infrared absorbing material,
The fields such as chemical industry, electronics, food, biology, medical science have broad application prospects.Therefore, the system of metal oxide nano-material
Standby technology turns into study hotspot.Currently, scientific worker has been developed that diversified metal oxide nano-material preparation side
Method, can be generally divided into solid phase method, liquid phase method and vapor phase method from build environment, specific to technology application, and including colloidal sol-solidifying
It is glue method, alkoxide hydrolysis, forced water solution, the gas-phase decomposition method of solution, wet chemical methods, microemulsion method, laser technology, micro-
Wave radiation technology, ultrasonic technique, AC electrodeposition technology, supercritical fluid drying technology, nonaqueous solvents hydrothermal technique etc..So
And, there is the defects such as reaction reagent poisonous and harmful, high cost, operational sequence are complicated, product is unstable in prior art, limit it
Further genralrlization application, the particularly use of material volume production.
The content of the invention
The technical problem to be solved in the present invention, is to provide a kind of preparation method of metal oxide nano ball.
What the present invention was realized in：A kind of preparation method of metal oxide nano ball, including herein below：In an electricity
In solution groove, anode is Pt pieces, and negative electrode is wire, and electrolyte uses high conductivity salting liquid, anode and negative electrode immersion electrolyte
Area ratio be anode：Negative electrode=20：1；
Using the Iarge Power DC Voltage Regulator of continuously adjustabe, by progressively high voltage, form plasma in negative electrode and put
Electricity, while forming sediment in the solution, sediment is purified, that is, obtain metal oxide nano ball.
Further, the negative electrode is the metal material corresponding to the metal oxide nano ball.
Further, the electrolyte is the NH of 3mol/L4NO3Solution.
Further, the voltage of the D.C. regulated power supply can be adjusted continuously between 0-200V, and maximum current is
10A。
Further, it is described by progressively high voltage, plasma discharge is formed in negative electrode, specially：
Voltage is increased since open-circuit voltage values with the speed of 1V/s, and finally terminal voltage stabilization is discharged in 100V.
The advantage of the invention is that：Participated in without poisonous and harmful chemical reagent, with low cost, simple to operate, material yield is high,
Expansibility is strong, is had a extensive future in industrial production.
Brief description of the drawings
The present invention is further illustrated in conjunction with the embodiments with reference to the accompanying drawings.
Fig. 1 is the structural representation of electrolysis unit in the present invention.
Fig. 2 is TiO in the present invention2The SEM of nanosphere overall (a) and a diameter of 2.7 μm of single particles (b) schemes.
Fig. 3 is TiO in the present invention2The XRD of nanosphere.
Fig. 4 is TiO in the present invention2The EDX collection of illustrative plates of nanosphere.
Specific embodiment
Refer to shown in Fig. 1, a kind of preparation method of titanium oxide nanosphere, by an Iarge Power DC Voltage Regulator and
One electrolytic cell constitutes electrolysis unit, and the voltage of power supply can continuously be adjusted between 0-200V, and maximum can bear electric current and be
10A.Anode uses Pt pieces, prevents anode to be dissolved in discharge process, and negative electrode is to prepare corresponding to titanium oxide nanosphere
Wire is Ti, and purity is 99.9%.Surface area in anode immersion electrolyte should as far as possible be more than negative electrode, the surface at the two poles of the earth
Product ratio about 20:1, electrolyte uses the NH of 3M4NO3Solution.The voltage at electrolytic cell two ends since open-circuit voltage values (about 0V),
Increased with the speed of 1V/s, under normal temperature, when terminal voltage reaches 25V or so, negative electrode starts electric discharge, and terminal voltage jumps to one immediately
Individual high value 90V, is discharged terminal voltage stabilization in 100V or so by regulation power supply.With the carrying out of electric discharge, electrolyte
Become muddy, obvious precipitation occurs in bottom of electrolytic tank, after experiment terminates, precipitation is repeatedly centrifuged purification, obtains final product titanium
Oxide nano sphere.
Obtained TiO2Nanosphere, SEM (SEM) photo of its pattern is as shown in Fig. 2 SEM figures show this
The diameter of a little spheric granules micron from below 100nm to hundreds of, wherein nano level particle occupies the overwhelming majority, averagely
Size is about in 500nm or so.
The present invention is using X-ray diffraction spectrum (XRD) and X-ray energy spectrometer (EDX) to particle TiO2The composition of nanosphere enters
Row is characterized, as a result as shown in Figure 3, Figure 4.The XRD spectrum of Fig. 3 shows TiO of the nanosphere by three types2Phase composition, respectively
Rutile Type, Anatase, and Anoxic Phase.Wherein, the composition of Anoxic Phase may be Ti10O19,Ti5O9Or Ti3O5This kind of phase
Than the TiO measured in conventional chemical2There is the thing phase of oxygen atom vacancy.The EDX collection of illustrative plates of Fig. 4 sets forth particulate samples and be placed in
Clean silicon chip (curve that mark B is referred to) in the case of (curve that mark A is referred to) and n.s presence is cleaned on silicon chip
Substrate collection of illustrative plates.By both contrasts it can be found that spheric granules is mainly made up of two kinds of elements of Ti and O, so as to confirm institute
The product for obtaining is TiO2Nanosphere.
Other experiment conditions and above-mentioned preparation TiO2Nanosphere is identical, using different cathode materials, can obtain difference
Metal oxide nano ball, such as using Al as negative electrode, can obtain with Al2O3Be the nanosphere of main component, using Cu as
Negative electrode, can obtain Cu2(OH)3NO3Nanosphere, using Fe as negative electrode, can obtain FeO, Fe2O3、Fe3O4The iron oxygen of blending constituent
Compound nanosphere.It follows that the present invention has universal applicability and scalability to preparing metal oxide nano ball.
The present invention has advantages below：
1st, method is simple, convenient, environmental protection, and the apparatus structure for being used is simple, with low cost, and preparation manipulation process is convenient,
Poisonous and harmful chemical reagent is not used；
2nd, nanosphere prepares yield greatly, TiO in testing as described above2The preparation yield of nanosphere can reach 50mg/min；
3rd, the present invention metal not high to fusing point has general applicability, and scalability is strong, using Ti, Al, Cu, Fe etc. no
Same metallic cathode material, can obtain different metal oxide nano balls.
4th, the present invention is that a kind of effective metal oxide nano ball is prepared and doping vario-property means, and experiment finds,
Plasma discharge high temperature quenching effect of lysigenous metallic particles when entering into electrolyte, for nanosphere it is final into
Divide and structure serves important modified and chanza.Composition in solution, it is easy to nanometer is incorporated into quenching process
In ball, such as Cu used as negative electrode, NH4NO3During as electrolyte, the nanosphere composition of generation is Cu2(OH)3NO3Rather than CuO.
By changing bath composition, modified, this doping vario-property can be doped to the metal oxide component and structure that generate
Response characteristics to light, catalysis characteristics of metal oxide nano ball etc. can be improved.
Claims (5)
1. a kind of preparation method of metal oxide nano ball, it is characterised in that：Including herein below：In an electrolytic cell, sun
Extremely Pt pieces, negative electrode is wire, and electrolyte uses high conductivity salting liquid, and the area ratio of anode and negative electrode immersion electrolyte is
Anode：Negative electrode=20：1；
Using the Iarge Power DC Voltage Regulator of continuously adjustabe, by progressively high voltage, plasma discharge is formed in negative electrode, together
When form sediment in the solution, sediment is purified, that is, obtain metal oxide nano ball.
2. the preparation method of metal oxide nano ball as claimed in claim 1, it is characterised in that：The negative electrode is the gold
Metal material corresponding to category oxide nano sphere.
3. the preparation method of metal oxide nano ball as claimed in claim 1, it is characterised in that：The electrolyte is
The NH of 3mol/L4NO3Solution.
4. the preparation method of metal oxide nano ball as claimed in claim 1, it is characterised in that：The D.C. regulated power supply
Voltage can continuously be adjusted between 0-200V, maximum current is 10A.
5. the preparation method of metal oxide nano ball as claimed in claim 1, it is characterised in that：It is described by progressively increasing
Voltage, forms plasma discharge, specially in negative electrode：
Voltage is increased since open-circuit voltage values with the speed of 1V/s, and finally terminal voltage stabilization is discharged in 100V.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107541746A (en) * | 2017-09-13 | 2018-01-05 | 西北师范大学 | The method that a kind of liquid phase cathode glow discharging plasma of sacrificial anode leaf prepares nano tungsten trioxide |
| WO2021104533A1 (en) * | 2019-11-25 | 2021-06-03 | 华南理工大学 | Quenching modification method for improving metal oxide electro-catalytic performance, and prepared metal oxide electro-catalyst and use |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106191902A (en) * | 2016-07-28 | 2016-12-07 | 北京科技大学 | A kind of method preparing hydrogen doping oxide ceramics micro Nano material |
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2017
- 2017-05-02 CN CN201710300029.5A patent/CN106929876A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106191902A (en) * | 2016-07-28 | 2016-12-07 | 北京科技大学 | A kind of method preparing hydrogen doping oxide ceramics micro Nano material |
Non-Patent Citations (4)
| Title |
|---|
| ZHAN WU等: "Titanium oxide nanospheres:preparation, characterization,and wide-spectral absorption", 《PHYS.STATUS SOLIDI A》 * |
| ZHI-KUN ZHANG等: "Plasma-electrolysis synthesis of TiO2 nano/microspheres with optical absorption extended into the infra-red region", 《CHEM. COMMUN.》 * |
| ZHI-KUN ZHANG等: "Preparation, characterization and catalytic property of CuO nano/microspheres via thermal decomposition of cathode-plasma generating Cu2(OH)3NO3 nano/microspheres", 《JOURNAL OF COLLOID AND INTERFACE SCIENCE》 * |
| 李兆虎等: "阴极等离子体电解法制备氧化铝纳米颗粒", 《物理化学学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107541746A (en) * | 2017-09-13 | 2018-01-05 | 西北师范大学 | The method that a kind of liquid phase cathode glow discharging plasma of sacrificial anode leaf prepares nano tungsten trioxide |
| WO2021104533A1 (en) * | 2019-11-25 | 2021-06-03 | 华南理工大学 | Quenching modification method for improving metal oxide electro-catalytic performance, and prepared metal oxide electro-catalyst and use |
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Application publication date: 20170707 |