CN105753069B - A kind of ball shaped nano mixed oxide（SiO2‑Fe2O3）The synthetic method of powder - Google Patents
A kind of ball shaped nano mixed oxide（SiO2‑Fe2O3）The synthetic method of powder Download PDFInfo
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- CN105753069B CN105753069B CN201610137140.2A CN201610137140A CN105753069B CN 105753069 B CN105753069 B CN 105753069B CN 201610137140 A CN201610137140 A CN 201610137140A CN 105753069 B CN105753069 B CN 105753069B
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- C01G49/00—Compounds of iron
- C01G49/0018—Mixed oxides or hydroxides
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- 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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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
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Abstract
A kind of ball shaped nano mixed oxide（SiO2‑Fe2O3）The synthetic method of powder, is related to a kind of nanometer of synthetic method of mixed oxide, the present invention that confined explosion reaction tube is evacuated using vavuum pump, is passed through mixed gas as explosive source from air guide port, and inject SiCl to charging aperture4Solution, is then heated using the electric heater unit of explosive reaction pipe outer wall, and treating that temperature reaches ensures SiCl4Closed when solution is gasified totally, using gas in spark ignition pipe, high temperature, high pressure, high velocity environment are produced by Gaseous Detonation, promoted precursor aqueous solution and iron plate that chemical reaction quickly occurs with mixed gas and directly generate nanometer spherical mixed oxide（SiO2‑Fe2O3）Powder.The method have the advantages that simple to operate, reaction unit and course of reaction is relatively inexpensive, response parameter controllable, energy saving, can continuous prodution, its spherical nanoparticle good dispersion, stable crystal form, well mixed, ratio is adjustable.
Description
Technical field
The present invention relates to a kind of nanometer of synthetic method of mixed oxide, more particularly to a kind of ball shaped nano mixed oxidization
Thing（SiO2-Fe2O3）The synthetic method of powder.
Background technology
Used as a kind of preferable inorganic nano magnetic material and optical material, nano-sized iron oxide not only has nano material
General character（Dimensional effect, skin effect and quantum tunneling effect）, while have the superparamagnetism that magnetic oxide is showed, by
It is widely used in the fields such as catalysis, anti-corrosion, pigment, ultraviolet radiation absorption, magnetic recording, magnetic probe and biomedicine.Nano oxygen
Changing iron has tempting magnetic and optical characteristics, but its nano particle bad dispersibility, and the activity of grain surface molecule is higher, easily
Generation is condensed and is grown, so as to lose good magnetic effect.Nano-meter SiO_22Had porous network structure, and chemical property and
Heat endurance is good, is commonly used for the disperse matrix of nano particle.If by magnetic nanoparticle（Fe2O3）It is distributed to nonmagnetic exhausted
Edge matrix of oxide（SiO2）The mixing nano material of middle composition（Fe2O3-SiO2）, can effectively prevent nanometer Fe2O3Reunion
Effect, improves its phase transition temperature, and also improves its single dispersing Jie while the characteristic of original nano magnetic material is saved
The dispersiveness and the assembling characteristic of composite nano materials of matter, make it with more extensive.At present, Fe2O3/ SiO2Nanometer mixing oxygen
The preparation of compound powder has been reported.Nanometer α-Fe2O3/SiO2With prominent heat endurance and gas sensing property, to common flammable
Gas and toxic gas have the sensitiveness of height.Optically, it is made using its absorbent properties to ultraviolet spectrogram ultraviolet
Line absorption film.As good nano magnetic particle, γ-Fe2O3/ SiO2Good biocompatibility is shown, in magnetic field
In the presence of can be oriented operation, be commonly used for magnetic field control material and biological targeting medicament carrier.
In nanometer Fe2O3-SiO2In the preparation technology of mixed oxide powder, generally using inorganic molysite solution (Fe
(NO3)3·9H2O、FeCl3·6H2O、Fe(ClO3)3), urea iron（[Fe(CON2H4)6](NO3)3）With iron oxide red (Fe2O3) make
It is source of iron and tetraethyl orthosilicate（TEOS）It is physico by sol-gel, forced hydrolysis, co-deposition, microemulsion, Hydrothermal Synthesiss etc.
Method is synthesized.Due to the shortcomings of preparation technology is complicated, the reaction time is long and reaction condition is difficult to control to so that prepared
Nano composite oxide powder bad dispersibility, easily reunite, crystal formation distortion and the difficult control of crystalline phase, the shortcomings of mixed proportion difficult control.
The content of the invention
It is an object of the invention to provide a kind of ball shaped nano mixed oxide（SiO2-Fe2O3）The synthetic method of powder,
The method synthesizing spherical SiO that the method is exploded by gas phase2-Fe2O3Nanometer mixed oxide powder, realizes being held under optimum condition
Continuous production ball shaped nano mixed oxide（SiO2-Fe2O3）Powder, can continuously be produced under identical operating mode, be a kind of warp
Ji, environmental protection, stabilization, the preparation method of the adjustable ball shaped nano mixed oxide powder of ratio.
The purpose of the present invention is achieved through the following technical solutions：
A kind of ball shaped nano mixed oxide（SiO2-Fe2O3）The synthetic method of powder, methods described includes procedure below：
Confined explosion reaction tube is evacuated using vavuum pump, mixed gas are passed through as explosive source from air guide port, and
SiCl is injected to charging aperture4Solution, is then heated using the electric heater unit of explosive reaction pipe outer wall, treats that temperature reaches really
Protect SiCl4Closed when solution is gasified totally, using gas in spark ignition pipe, high temperature, high pressure, height are produced by Gaseous Detonation
Fast environment, promotes precursor aqueous solution and iron plate that chemical reaction quickly occurs with mixed gas and directly generates nanometer spherical mixed oxide
（SiO2-Fe2O3）Powder.
A kind of described ball shaped nano mixed oxide（SiO2-Fe2O3）The synthetic method of powder, the mixed gas are
The mass ratio 0. 094 ~ 0.167 of hydrogen-oxygen mixed gas, control hydrogen and oxygen.
A kind of described ball shaped nano mixed oxide（SiO2-Fe2O3）The synthetic method of powder, the precursor solution
It is SiCl4 solution, its mass percentage concentration is 90% ~ 99.5%.
A kind of described ball shaped nano mixed oxide（SiO2-Fe2O3）The synthetic method of powder, it is described in explosive reaction
Inside pipe wall attaches one layer except the tagger of oxide layer provides source of iron.
A kind of described ball shaped nano mixed oxide（SiO2-Fe2O3）The synthetic method of powder, the sparking mode is
Electric ignition is detonated, the 2200 ~ 5000V of crest voltage of detonation, and detonation can be controlled in 50 ~ 200J.
A kind of described ball shaped nano mixed oxide（SiO2-Fe2O3）The synthetic method of powder, the confined explosion is anti-
Pipe outer wall is answered closely to be heated one layer of heating tape of cladding, and the initial temperature for controlling detonation to react equipped with digital display temperature-control equipment
Degree, it is 25 ~ 300 DEG C to control initial temperature.
A kind of described ball shaped nano mixed oxide（SiO2-Fe2O3）The synthetic method of powder, the conduit upper pair
Claim to set three pressure sensors, and connect pressure detecting system, to peak in the explosive reaction pipe in whole detonation course of reaction
Duty pressure carries out real-time detection；It is 1.0 ~ 2.0MPa to control the surge pressure in detonation reaction tube.
A kind of described ball shaped nano mixed oxide（SiO2-Fe2O3）The synthetic method of powder, the utilization XRD,
The characterization methods such as XRF, TEM enter to crystallite dimension, crystalline phase composition, shape characteristic of crystal grain of product synthesized by claim 1 etc.
Row is characterized, gained mixed oxide（SiO2-Fe2O3）The particle diameter of powder is in 50 ~ 120nm.
Advantages of the present invention is with effect：
1. the present invention is utilizing SiCl4Solution prepares Nano-meter SiO_2 as precursor solution Gaseous Detonation2Principle on, quick-fried
The tagger of removing oxide-film is set in fried reaction tube to provide nanometer Fe2O3Source of iron, by gas phase explode method synthesize ball
Shape SiO2-Fe2O3Nanometer mixed oxide powder.Devise a set of gas phase explosive reaction device（Fig. 1）To be tested and be controlled
Detonation parameter.
2. the detonation wave and the interior strong Dynamic Coupling mechanism for chemically reacting of explosive reaction pipe for being produced according to Gaseous Detonation,
High temperature, high pressure and high speed communication process that continual and steady maintenance detonation is reacted.Promote reaction using the powerful Explosive Energy of release
Thing quickly generates nano particle, and detonation gas bulking effect is sufficiently mixed nano particle, forms stabilization, well mixed nanometer
Mixed oxide powder.By changing detonation response parameter（Initial temperature, pressure and ignition energy etc.）With initial reactant concentration
And explosion gas matches to control crystallite dimension, crystalline phase composition and the mixed proportion of nano particle.Realize continuing under optimum condition
Production ball shaped nano mixed oxide（SiO2-Fe2O3）Powder.
3. according to gas combustion explosion principle, the Explosive Energy of gas phase blast release can activate chemical reaction to the present invention, while
Chemical reaction releases energy and maintains the propagation of explosion wave in turn, stabilizes it propagation.The nanometer mixed oxidization of generation
Thing has little time to reunite, the ball shaped nano powder of the good dispersion that is easy to get.
4. the present invention can control the discharged energy of blast by changing the different proportion of hydrogen-oxygen mixed gas, from
And influence the crystal structure and crystal formation of nanometer mixed oxide to constitute, also can be anti-by changing the concentration and detonation of precursor aqueous solution
The initial environment (initial temperature and pressure) answered realizes the control to nanometer mixed oxide.To reach under optimal operating mode
The synthesis of nanometer mixed oxide is carried out, the ratio to each composition in control product is realized.
5. the product purity that prepared by the present invention is high, is avoided that impurity during using conventional explosives explosion method synthetising nanometre powder body
Introduce（Mainly carbon）.With simple to operate, course of reaction it is rapid, experimental rig is simple, required raw material is cheap and can be identical
The advantages of continuously being produced under operating mode, is a kind of suitable economic and environment-friendly nano-mixture（SiO2-Fe2O3）The method of powder.
Brief description of the drawings
Fig. 1 is explosive reaction pipe schematic diagram of the invention；
Fig. 2 is present invention synthesis nanometer mixed oxide（SiO2-Fe2O3）Powder XRF analysis result figure；
Fig. 3 is two kinds of nanometer mixed oxides of size of the invention（SiO2-Fe2O3）Powder TEM schemes.
Specific embodiment
With reference to embodiment, the present invention is described in detail.
The present invention proposes one kind using gas phase blast to prepare ball shaped nano mixed oxide（Fe2O3-SiO2）Powder
Synthetic method, and designed, designed explosive reaction pipe（Such as Fig. 1）Gas phase explosive reaction is tested, control explosive reaction ginseng
Number.Gas phase blast prepares Nano-meter SiO_22The characteristic of powder is to utilize SiCl4Solution as presoma, using hydrogen-oxygen mixed gas as
Explosive source, in the case where insulation and temperature control system and pressure capsule system are configured and monitor to initial temperature and pressure environment, profit
Detonated with spark ignition, make confined explosion reaction tube implosion source gas superquick action, discharge substantial amounts of explosion energy activation not
The quick-fried source gas of reaction zone, promotes precursor solution fast reaction to generate Nano-meter SiO_22Powder, and gradually grow up to form particle, sink
Product is on interior test tube wall.
The present invention is in explosive reaction inside pipe wall to add one layer of sheet iron for removing oxide film dissolving in this experimental basis to carry
For nanometer Fe2O3Source of iron, make tagger in the environment of reacting the high temperature for producing, high pressure and high density by Gaseous Detonation in pipe
Surface iron molecule reacts with explosive source gas Quick Oxidation, and and Nano-meter SiO_22Particle is fully mixed in the expansion process of detonation gas
Close, ultimately form stabilization, well mixed ball shaped nano mixed oxide（Fe2O3-SiO2）Powder.
In order to solve this nanometer of technical problem of mixed oxide gas phase blast synthetic method, it is achieved it, therefore
Devise gas phase explosive reaction pipe as shown in Figure 1.The device specifically includes 11 parts, wherein：1 quick-fried source H2 gas bombs, 2
Quick-fried source O2 gas bombs, 3 vavuum pumps, 4 valves, 5 fire holes, 6 charging apertures, 7 pressure sensors, 8 reactors, 9 cables, 10 vacuum
Table, 11 chlorine absorbers；The inwall of reactor 8 is cased with one layer of tagger to provide source of iron；It is controlled by pressure-reducing valve respectively, is used
Gas hose accesses the charging connector on wireway；Vavuum pump 3, vacuum meter 10 and valve 4 are used for extracting vacuum and control pressure sets
It is standby, it is connected with reaction unit with rubber hose and screw socket single head respectively；In view of clean environment firendly, with rubber hose by chlorine absorber
11 connect air guide tube end, and a small amount of chlorine to being produced after reaction is collected.In order to consider Gaseous Detonation reaction unit
Security, accuracy and operability, are respectively provided with accurate ball valve, controlling switch at all interfaces for external devices.The present invention is main
The experiment flow wanted is as follows：To be evacuated in reactor 8 by vavuum pump 3, from quick-fried source H2 gas bombs 1 and quick-fried source O2 gases
Steel cylinder 2 is passed through hydrogen and oxygen, while injecting SiCl into container from charging aperture 64Solution, by cable 9 to explosive reaction pipe
Interior mixture is heated, and controls blast initial temperature with temperature control device, it is ensured that SiCl4Solution can be gasified totally,
Can uniformly mix with explosion gas.During temperature-controlling system set temperature value to be achieved, electric spark point is passed through at fire hole 5
Fiery mode carries out ignition and detonation, and gas explosion promotes SiCl in activation pipe4Steam and iron plate chemically react with explosion gas
Generation ball shaped nano mixed oxide（SiO2-Fe2O3）Powder.Deposition is stood after the completion of detonation after 10 ~ 20 minutes, treats that temperature drops
During to normal temperature, opening flanged plate carries out powder collection.
Embodiment
From the thick homogeneous taggers of 0.7mm, cut and grown into 1300mm, the rectangle iron plate of a width of 480mm is utilized
Commercial concentration is 30% acid wash passivation liquid（Main component is HF）Clean to remove the oxide-film and impurity on iron plate surface.With length
While rolling rectangle iron plate for axle forms cylindrical shape, it is inserted in self-control detonation reaction tube and it is close to completely in detonation reaction tube
Wall.
Experimental provision is connected as shown in Figure 1, all valves of detonation reaction tube both sides are closed, and allows detonation reaction tube to be formed
Closed environment, connects model V-i120SV at vavuum pump 3, and the speed of exhaust is 3.6m3The vavuum pump of/h, and open vacuum meter
（-0.1~0.5MPa）Place's valve, switches on power and starts to vacuumize Detonation Tube.After about extracting 4 min, vacuum list index is observed
Registration is -80KPa, and continues to vacuumize, and pointer registration is basically unchanged, then it is assumed that has been vacuum environment in detonation reaction tube, has closed
Close vacuum meter valve.
Successively the hydrogen and oxygen bottle valve connect at quick-fried source H2 gas bombs 1 and quick-fried source O2 gas bombs 2 are opened respectively
Door, by H2:O2=2:1 to the H that 0.04 MPa is passed through in detonation reaction tube2With the O of 0.02 MPa2, cylinder valve is utilized during ventilation
On the pressure-reducing valve that is connect carry out Stress control.After having led to gas, it is 99.5% (AR's) to extract 2 ml purity using syringe
SiCl4Solution, in the charging aperture injection detonation reaction tube from charging aperture 6, turns off the accurate ball valve at charging aperture.
220 V are wrapped with detonation reaction pipe outer wall, power is the glass fibre heating tape of 1000 W, and connects commercially available Yao Yi
The digital display temperature-control equipment of board.The initial temperature for first setting detonation is 150 DEG C, switches on power and is heated.Treat that temperature reaches 150
After DEG C, stop heating and deenergization.After checking experiment device ensures safety, using the FD150 types electricity connected at fire hole 5
Appearance formula exploder, ignition and detonation is carried out using electric spark formula.
After the completion of reaction, allow detonation reaction tube to stand 10 ~ 15 min, treat that the solid powder of generation in detonation reaction tube is complete
It is complete deposit and be cooled to normal temperature after, the valve for opening exhaust collection steel cylinder carries out exhaust collection.After pressure gauge registration stabilization, beat
Both sides flanged plate is opened, detonation product is collected.Filtered using pore sieve, then cleaned with distilled water, be finally evaporated
To dry nano-powder.
X-ray diffraction analysis (XRD) is carried out to adulterated powder using X-ray, obvious Fe is as a result found2O3Diffraction maximum,
Fe is calculated by Scherrer formula2O3Crystallite dimension be 68.9 nm, and the SiO in products therefrom2It is noncrystalline state,
Form disperse peak.Analyzing (XRF) by X-ray fluorescence spectra carries out constituent analysis (Fig. 2) to products therefrom, as a result finds nanometer
The mass ratio and mol ratio of silica are accounted for respectively:20.5% and 39.7%, the quality point of nano-sized iron oxide with mol ratio than distinguishing
For:76.3% and 55.6%.Morphology characterization (Fig. 3) is carried out to product using transmission electron microscope (TEM), nanometer mixed oxidization is as a result found
Thing（SiO2-Fe2O3）Powder granule is spherical, and preferably, crystal grain size is in 50 ~ 120nm or so for the dispersiveness of crystal.
Claims (4)
1. a kind of ball shaped nano mixed oxide SiO2-Fe2O3The synthetic method of powder, it is characterised in that methods described include with
Lower process：
Confined explosion reaction tube is evacuated using vavuum pump, Hydrogen Oxygen mixed gas is passed through as explosive source from air guide port,
The mass ratio 0. 094 ~ 0.167 of control hydrogen and oxygen；And inject SiCl to charging aperture4Solution, SiCl4The quality percentage of solution
Concentration is 90% ~ 99.5%, and one layer is attached except the tagger of oxide layer provides source of iron, conduit upper in explosive reaction inside pipe wall
Three pressure sensors are symmetrical arranged, and connect pressure detecting system, in the explosive reaction pipe in whole detonation course of reaction
Surge pressure carries out real-time detection；The surge pressure in detonation reaction tube is controlled for 1.0 ~ 2.0MPa, using explosive reaction pipe
The electric heater unit of outer wall is heated, and treating that temperature reaches ensures SiCl4Closed when solution is gasified totally, using spark ignition
Gas in pipe, high temperature, high pressure, high velocity environment are produced by Gaseous Detonation, promote precursor aqueous solution and iron plate quick with mixed gas
Generation chemical reaction directly generates nanometer spherical mixed oxide SiO2-Fe2O3Powder.
2. a kind of ball shaped nano mixed oxide SiO according to claim 12-Fe2O3The synthetic method of powder, its feature
It is that sparking mode is detonated for electric ignition, the 2200 ~ 5000V of crest voltage of detonation, detonation can be controlled in 50 ~ 200J.
3. a kind of ball shaped nano mixed oxide SiO according to claim 12-Fe2O3The synthetic method of powder, its feature
It is confined explosion reaction pipe outer wall is closely heated one layer of heating tape of cladding, and is controlled equipped with digital display temperature-control equipment
The initial temperature of detonation reaction processed, it is 25 ~ 300 DEG C to control initial temperature.
4. a kind of ball shaped nano mixed oxide SiO according to claim 12-Fe2O3The synthetic method of powder, its feature
Be, using XRD, XRF, TEM characterization method to the crystallite dimension of product synthesized by claim 1, crystalline phase composition, crystal grain shape
Looks feature is characterized, gained mixed oxide SiO2-Fe2O3The particle diameter of powder is in 50 ~ 120nm.
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| CN108394885B (en) * | 2018-03-26 | 2021-03-26 | 大连理工大学 | Method for synthesizing solid carbon quantum dots by gas-phase detonation |
| CN108587367A (en) * | 2018-04-19 | 2018-09-28 | 杨帮燕 | A kind of preparation method of film printing coating |
| CN109128219A (en) * | 2018-09-30 | 2019-01-04 | 大连理工大学 | A kind of method that Gaseous Detonation method synthesizes carbon-based cobalt-copper alloy nano material |
| CN112111181B (en) * | 2020-10-22 | 2022-01-11 | 南京森峰科技有限公司 | Carbon black preparation device and method based on explosion method |
| CN113359903B (en) * | 2021-06-25 | 2022-07-15 | 中国科学技术大学 | Heating method for detonation pipeline |
| CN113457570A (en) * | 2021-08-06 | 2021-10-01 | 甘肃宁氏实业有限责任公司 | High-energy-rate synthetic material gas-phase preparation device and method |
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