CN101219776B - Method and device for manufacturing non-glomeration nano-oxide powder body - Google Patents
Method and device for manufacturing non-glomeration nano-oxide powder body Download PDFInfo
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- CN101219776B CN101219776B CN2008100329742A CN200810032974A CN101219776B CN 101219776 B CN101219776 B CN 101219776B CN 2008100329742 A CN2008100329742 A CN 2008100329742A CN 200810032974 A CN200810032974 A CN 200810032974A CN 101219776 B CN101219776 B CN 101219776B
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Abstract
The invention relates to a method and a device for preparing nanometer oxide powders without agglomeration. The method combines an electron spraying and a combustion method, separates nanometer particles by charging the surfaces of aerosol particles which are generated during nanometer combustion with the same charge, and overcomes hard agglomeration existing in the combustion method. The preparation device comprises a combustor, a liquid pump, a bracket and a collecting board; an outlet of the liquid pump is connected with an electronic sprayer through a tube; a nozzle of the electronic sprayer aims at an inlet of the combustor, and an outlet of the combustor aims at the collecting board. The method and device of the invention can prepare and obtain the nanometer oxide powders without hard agglomeration.
Description
Technical field
The present invention relates to a kind of preparation method and device of non-glomeration nano-oxide powder body.
Background technology
At present some prepare the method for nano oxide powder, as the precipitator method, and sol-gel method, combustion method, hydrothermal method, ultrasonic spray pyrolysis, the microwave-assisted pyrolysis, antiphase emulsifiable method, spray pyrolysis etc. fail to solve well the problem of hard aggregation always.In addition, the preparation of the nano-oxide solid solution powder of hard aggregation-free is a task of difficulty more.
For avoiding the formation of hard aggregation, Xia etc. propose the aerosol that salt is added in pyrolysis.Since salt separate out the nano particle that wraps generation, thereby avoid the formation of hard aggregation.Shen etc. then directly sneak into salt in the powder stock before pyrolysis when pyrolysis prepares nano-ZnO, have to a certain degree reduced the formation of hard aggregation.Propositions such as Chen Weifan adopt salt hydrotropy liquid combustion method to prepare the method for high specific surface cerium nano-powder.Promptly in traditional solution combustion method, introduce KCl to form the salt deposit parcel of nano particle, make the product specific surface area that obtains increase by 10 times.But, the also fine far away solution of hard aggregation problem.
Recently, be the sosoloid nano-powder of preparation hard aggregation-free, Japanese scholar proposes " the synthetic multi-component oxide nano-powder of nanometer blast ", and prepares the less CeO of hard aggregation
2/ 20Gd sosoloid nano-powder.The main process of this method comprises that precipitation generates nano-reactor, and is synthetic and the explosive RDX nano-reactor of packing into, and heating RDX blast generation High Temperature High Pressure obtains CeO after the blast
2/ Gd sosoloid nano-powder.This method is an impressive progress in the sosoloid nano powder preparation.Its main drawback is if the outer explosive RDX of nano-reactor does not clean up (in fact relatively difficulty), obtains the powder of hard aggregation after the blast probably, and the sosoloid nano-powder that obtains also needs thermal treatment to remove the blast residual component.
Summary of the invention
The objective of the invention is to defective, a kind of preparation method and device of non-glomeration nano-oxide powder body is provided, can prepare the nano oxide powder of hard aggregation-free at prior art.For achieving the above object, design of the present invention is:
In the present invention, be oxide compound and the oxide solid solution nano powder preparation method that develops a kind of effective hard aggregation-free, we combine electron spray(ES) (electrospraying) technology and combustion method synthetising nanometre powder body method, electron spray(ES)-nanometer the combustion method of the preparation nano oxide powder of applicant's proposition is improved in development, that is: obtain the charged submicron/micron order drop of uniform precursor solution (being the mixing solutions of metal salt solution and organic-fuel solution) by electron spray(ES), high temperature makes little drop solvent evaporation and secondary-atomizing during by burner, the metal salt solution that contains in little drop (as: Zn (NO
3)
2, Cu (NO
3)
2Deng ethanolic soln) and organic-fuel (as the ethanolic soln of glycine) become the dispersive charged aerosol, nanometer range takes place independently and acutely burns in each aerosol nanoparticles in the thermal-flame district, generate nm-class oxide powder.The like charges that gas that the nanometer burning produces and nano-powder have makes between the nano particle isolates, and collects the nm-class oxide powder that obtains hard aggregation-free at last.
Use precursor solution to prepare powder and must finish two tasks by electron spray(ES): the one, need to use carrier gas little drop that electron spray(ES) produces to be transported to a high-temperature zone by pipeline, make the solvent evaporation solute decompose the powder that obtains preparing.The 2nd, before using the carrier gas transportation, need neutralize little drip gauge surface charge, to avoid because the electrostatic repulsion between little drop excessively disperses drop, otherwise carrier gas can't transport these too the little drop of dispersive pass through pipeline.We propose to introduce burner and solve above-mentioned difficulties, have both utilized burner that presoma is decomposed, and make full use of the drip gauge surface charge and realize further atomizing little drop.
Flame method subject matter is that the powder hard aggregation that obtains is serious.Have only when precursor vapor concentration presoma drop very low or that introduce is tiny to arrive several microns, just be hopeful to overcome this difficulty.Someone proposes to adopt secondary-atomizing, but complex process needs CONTROL PROCESS very strictly.The flame atomizing method is metal salt solution (as: Zn (NO
3)
2) ethanolic soln when atomizing by pressurized air, igniting makes atomized liquid concurrent estranged the separating of burning make ultra-micro powder.Because the little drop of liquid in the fog is bigger, the powder hard aggregation is difficult to avoid in this method.We propose to obtain micron/submicron droplets by electron spray(ES), avoid little droplet collision to grow up by the drip gauge surface charge, and little drop is when the solvent evaporation volume-diminished, drip gauge surface charge repulsion can surpass surface tension, secondary-atomizing (Coulomb fission) takes place, obtain submicron and nano-liquid droplet, thereby solve the difficulty of above-mentioned flame method.
The burner of cylindrical structure is inboard to be pottery for stainless steel (maybe can switch on) is outer, the burner inboard is distributed with oxygen blast hole (can evenly upwards be blown into air or oxygen in case of necessity) from bottom to top successively, teasehole (pore is to supply with ethanol), demountable metal discharge fine needle (can produce and the identical electric charge in little drop surface), with in the oxygen blast hole of burner inner top side, so that outside burner outlet, obtain thermal-flame.As required, by changing ethanol feed rate and whether oxygen blast and blowing oxygen quantity size, the temperature distribution that the control burner is interior and the flame temperature at burner outlet place.We show in preliminary experiment, use ethanol to be fuel, and the outlet flame temperature has reached 700 ℃ when not oxygen blast, can reach 1100 ℃ during a small amount of oxygen blast.Therefore, organic-fuel such as glycine can complete reaction burn, and obtain oxide powder.In addition, according to the experiment situation, the burner inboard can have and the identical electric charge in little drop surface, to stop side contacts in little drop and the burner.Because ethanol and solvent burning can produce water vapour, may cause little drip gauge surface charge to be scattered and disappeared.The spray point of burner inboard can be given the water vapour charging (electrically identical with little drop surface) of ethanol and generation, in conjunction with the electric charge of burner inboard, can effectively slow down little drip gauge surface charge and scatter and disappear.
According to the foregoing invention design, the present invention adopts following technical proposals:
A kind of preparation method of non-glomeration nano-oxide powder body.It is characterized in that electron spray(ES) and combustion method are combined, the aerosol particle surface that the nanometer burning is produced has like charges and nano particle is separated, and overcomes the hard aggregation that occurs in the combustion method;
The concrete operations step is as follows:
1) precursor solution is carried out electron spray(ES), obtain charged submicron/micron order drop;
2) above-mentioned drop carries out high temperature evaporation and secondary-atomizing by the combustion chamber, burns in the thermal-flame district then, produces gas and nm-class oxide powder;
3) nm-class oxide powder that produces of above-mentioned burning has like charges and is isolated from each other between particle, adopts collecting board to collect, and obtains the nm-class oxide powder of hard aggregation-free.
Above-mentioned precursor solution is metal salt solution (0.05M-1M) and organic-fuel, and as the mixing solutions of the ethanolic soln (0.1M-5M) of glycine, its ratio is by volume: 1: 1-1: 5.
Above-mentioned metal salt solution is the ethanolic soln of the nitrate of Zn or Cu, and described organic-fuel solution is the ethanolic soln of glycine.
A kind of preparation facilities of non-glomeration nano-oxide powder body, be applied to above-mentioned preparation method, comprise burner, liquor pump, support and collecting board, it is characterized in that described liquid pump outlet is by EFI day with fog of pipe connection, its spout is aimed at the import of burner, and collecting board is aimed in the outlet of burner.
The jet pipe of above-mentioned EFI day with fog connects the positive pole of power supply, and places the ring electrode in jet pipe the place ahead to connect the negative pole of power supply.
The structure of above-mentioned burner is: ceramic coat is being overlapped in a stainless steel lined outside, circumferentially uniform oxygen blast hole is all arranged in the upper and lower, circumferentially uniform teasehole is arranged on oxygen blast hole, bottom, the inwall fixed installation of the stainless steel lined on teasehole is uniform metal fine needle circumferentially, described stainless steel lined is by the positive pole of wire connecting power, and described collecting board is by the negative pole of wire connecting power.
Above-mentioned support fixedly mounts EFI day with fog, burner and collecting board from top to bottom successively.
The present invention compared with prior art, have following conspicuous outstanding substantive distinguishing features and remarkable advantage: method of the present invention adopts electron spray(ES) and combustion method to combine, the aerosol particle surface that the nanometer burning is produced has like charges and nano particle is separated, overcome the hard aggregation that occurs in the combustion method, and the reaction in thermal-flame, further residue is removed in thermal treatment.Apparatus structure of the present invention rationally, compact, simple, be easy to make, cost is low.
Description of drawings
Fig. 1 is the preparation facilities structure principle chart of a non-glomeration nano-oxide powder body of the present invention.
Fig. 2 is the structural representation of the burner among Fig. 1.
Fig. 3 is an A-A place sectional view among Fig. 2
The conical jet of Fig. 4 alcohol fuel.
Fig. 5 is a preparation method's of the present invention schema.
Fig. 6 is the stereoscan photograph figure with the ZnO nano-powder of preparation method's preparation of the present invention.
Embodiment
A preferred embodiment of the present invention accompanying drawings is as follows:
Referring to Fig. 4 and Fig. 1, the preparation method of this non-glomeration nano-oxide powder body, the details flow process is as follows:
Electron spray(ES)-nanometer flame method uses common inorganic salt to be raw material, need not to prepare complicated chemical processes such as colloidal sol, has simply advantage applied widely.Can obtain the powder that corresponding chemical is formed by changing the solute proportioning; Can regulate prepared oxide powder particle diameter by changing solute concentration and electron spray(ES) processing parameter etc.In addition, can improve powder output by the method that adopts array.
It is as follows that present embodiment uses this method to prepare the process explanation of ZnO nano-powder, referring to Fig. 5,
1. compound concentration is the Zn (NO of 0.05M
3)
2Ethanolic soln.
2. with the speed of 38ml/h ethanol is advanced to burner with liquor pump, lights.
3. Zn (NO
3)
2Ethanolic soln and after the ethanolic soln (1M) of glycine mixes with 1: 1 volume ratio, release metal thin tube with another liquor pump with the constant speed of 1.0ml/h and enter highfield, at terminal stable conical jet, the realization electron spray(ES) of forming of metal thin tube.
4. charged little drop generation secondary-atomizing forms more small droplets in the burner.
5. under the high temperature, Zn (NO in little drop
3)
2Become charged nanometer aerosol with organic-fuel glycine drying or part drying.
6. nanometer aerosol particle generation nanometer range is acutely burnt in the thermal-flame, decomposes to generate nano ZnO powder.
7. collect on the water-cooled collecting board up, obtain the ZnO nano-powder of hard aggregation-free.Its stereoscan photograph is seen Fig. 6.
Use electron spray(ES)-nanometer flame method can prepare the oxide compound of most of kinds of other hard aggregation-frees and oxide solid solution nano-powder (as CuO, Y
2O
3Deng) process is the same.
Referring to Fig. 1, preparation facilities burner 4, liquor pump 10, support 8 and collecting board 7 that present embodiment uses, the outlet of described liquor pump 10 is by EFI day with fog 1 of pipe connection, and its spout is aimed at the import of burner 4, and collecting board 7 is aimed in the outlet of burner 4.The jet pipe of EFI day with fog 1 connects positive pole, and places the ring electrode 2 in jet pipe the place ahead to connect the negative pole of power supply.Referring to Fig. 2 and Fig. 3, the structure of burner 4 is: ceramic coat 15 is being overlapped in stainless steel lined 14 outsides, circumferentially uniform oxygen blast hole 11 is all arranged in the upper and lower, circumferentially uniform teasehole 12 is arranged on oxygen blast hole, bottom 11, the inwall fixed installation of the stainless steel lined 14 on teasehole 12 is uniform metal fine needle 13 circumferentially, described stainless steel lined 14 is by the positive pole of wire connecting power, and described collecting board 7 is by the negative pole of wire connecting power.The import 3 of combustion chamber below, the liquid fuel pump is connected the fuel aperture of burners 4 by pipeline 9, the outlet 6 of burner 4 is discharged the gas that the nanometer burning produces and the nm-class oxide powder 7 of band like charges up.Fig. 4 illustrates the alcoholic acid conical jet.
Claims (7)
1. the preparation method of a non-glomeration nano-oxide powder body; It is characterized in that electron spray(ES) and combustion method are combined, the aerosol particle surface that the nanometer burning is produced has like charges and nano particle is separated, and overcomes the hard aggregation that occurs in the combustion method; The concrete operations step is as follows:
A. precursor solution is carried out electron spray(ES), obtain charged submicron/micron order drop;
B. above-mentioned drop carries out high temperature evaporation and secondary-atomizing by the combustion chamber, burns in the thermal-flame district then, produces gas and nm-class oxide powder;
C. the nm-class oxide powder that above-mentioned burning produces has like charges and is isolated from each other between particle, adopts collecting board to collect, and obtains the nm-class oxide powder of hard aggregation-free.
2. the preparation method of non-glomeration nano-oxide powder body according to claim 1 is characterized in that described precursor solution is a metal salt solution, and its concentration is the mixing solutions of 0.05M～1M and organic-fuel, and its ratio is by volume: 1: 1～5.
3. the preparation method of non-glomeration nano-oxide powder body according to claim 2 is characterized in that described metal salt solution is the ethanolic soln of the nitrate of Zn or Cu, and described organic-fuel is the ethanolic soln of glycine, and its concentration is 0.1M～5M.
4. the preparation facilities of a non-glomeration nano-oxide powder body, be applied to the preparation method of non-glomeration nano-oxide powder body according to claim 1, comprise burner (4), liquor pump (10), support (8) and collecting board (7), the outlet that it is characterized in that described liquor pump (10) is by an EFI day with fog of pipe connection (1), its spout is aimed at the import of burner (4), and collecting board (7) is aimed in the outlet of burner (4).
5. the preparation facilities of non-glomeration nano-oxide powder body according to claim 4 is characterized in that the jet pipe of described EFI day with fog (1) connects positive pole, and places the ring electrode (2) in jet pipe the place ahead to connect the negative pole of power supply.
6. the preparation facilities of non-glomeration nano-oxide powder body according to claim 4, the structure that it is characterized in that described burner (4) is: ceramic coat (15) is being overlapped in a stainless steel lined (14) outside, circumferentially uniform oxygen blast hole (11) is all arranged in the upper and lower, circumferentially uniform teasehole (12) is arranged on oxygen blast hole, bottom (11), the inwall fixed installation of the stainless steel lined (14) on teasehole (12) is uniform metal fine needle (13) circumferentially, described stainless steel lined (14) is by the positive pole of wire connecting power, and described collecting board (7) is by the negative pole of wire connecting power.
7. according to the preparation facilities of claim 4 or 5 or 6 described non-glomeration nano-oxide powder bodies, it is characterized in that described support (8) fixedly mounts EFI day with fog (1), burner (4) and collecting board (7) from top to bottom successively.
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| CN2008100329742A CN101219776B (en) | 2008-01-23 | 2008-01-23 | Method and device for manufacturing non-glomeration nano-oxide powder body |
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| CN103935961B (en) * | 2014-04-21 | 2017-01-25 | 华侨大学 | Metallic oxide nano-powder preparation method capable of achieving large-scale production |
| WO2017129516A1 (en) * | 2016-01-27 | 2017-08-03 | Evonik Degussa Gmbh | Process for producing tungsten oxide and tungsten mixed oxides |
| CN106745194B (en) * | 2016-12-15 | 2017-12-29 | 西安航空学院 | The preparation method of ZnO hollow Nano particles |
| CN113830816A (en) * | 2021-04-28 | 2021-12-24 | 广东石油化工学院 | Process for synthesizing multi-metal nano oxide by using confined combustion effect in high-dispersion hot spot |
| CN114733474B (en) * | 2022-04-13 | 2023-05-16 | 清华大学 | Device for electrospray assisted atomization of flame synthesis functional nano particles |
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