CN107055606B - A kind of preparation method of red schorl phase titanium dioxide nano ball - Google Patents
A kind of preparation method of red schorl phase titanium dioxide nano ball Download PDFInfo
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- CN107055606B CN107055606B CN201710467017.1A CN201710467017A CN107055606B CN 107055606 B CN107055606 B CN 107055606B CN 201710467017 A CN201710467017 A CN 201710467017A CN 107055606 B CN107055606 B CN 107055606B
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Abstract
A kind of preparation method of red schorl phase titanium dioxide nano ball of the invention belongs to technical field of preparation for inorganic material.The preparation method have Ti electrode preparation, inflation, open plasma heating reaction, collect product, annealing and etc..The present invention has many advantages, such as that preparation process is simple, preparation time is short, it is environmental-friendly to prepare, yield is big and at low cost, the nanosphere structural stability of preparation is good, crystallinity is high, product purity is high, size distribution ranges are narrow, particle spherical surface is smooth, and monodispersity is good, can be used for rutile crystalline and the higher field of purity requirement.
Description
Technical field
The invention belongs to technical field of preparation for inorganic material, it particularly relates to a kind of red schorl phase titanium dioxide nano
The preparation method of ball.
Background technique
Nano-titanium dioxide mainly has three kinds of anatase, brockite and rutile crystal phases.Wherein, red schorl phase titanium dioxide
Nanostructure is due to, dielectric constant height stable with macroscopic property, refractive index height, excellent translucency and very strong ultraviolet light
Screening ability is widely used in electronics industry and coatings industry.Therefore, low cost, shape how to be prepared
Looks and the controllable pure phase rutile type nano of size have become the research hotspot in titanium dioxide field.
The prior synthesizing method of red schorl phase titanium dioxide nano particle mainly has liquid phase method and vapor phase method.Liquid phase method is main
It is current laboratory and industrial wide comprising preparation methods such as sol-gel method, liquid-phase precipitation method, solvent-thermal method and hydro-thermal methods
The preparation method of general use.Although the titanium dioxide nanoparticle of liquid phase method preparation has, diameter of particle size is controllable, synthesis is warm
Spend the advantages that lower, at low cost, but still have some still unsolved difficulties: 1) titanium source of liquid phase method is typically derived from four
The titaniferous chemical reagent such as titanium chloride or butyl titanate, and these reagents have the shortcomings that high price, high-risk, high toxicity,
Transport, uses and saves all that there is security risks.2) liquid phase method preparation process step is many and diverse, complicated for operation, time-consuming, preparation
Process is easy to produce pollution, poor repeatability.3) nanoparticle structure is not easy to control, and particle is easy to reunite, and hardly results in monodisperse
Nano particle.4) preparation process is readily incorporated impurity, hardly results in the higher Rutile Type of purity, and then influence final product
Performance.The titanium dioxide nanostructure of vapor phase method production is with crystal structure is good, crystal phase is with high purity, chemical activity is high, single
Good dispersion, few advantage of reuniting, have become the prefered method especially to the higher field of rutile quality requirements.To current
Until, although vapor phase method has made great progress, preparation cost is low, and preparation time is short, and simple process is reproducible, preparation
Environmental-friendly operation, the vapor phase method for being able to satisfy industrialization large-scale production still need further to be developed.
Accordingly, inexpensive, yield is big, the research and development of environmental-friendly and high-quality red schorl phase titanium dioxide nano particle,
Achieve the purpose that realize that nano material simply prepares and improve material property, explores greenization, the preparation of its material preparation method
The simplification of technique is imperative.
Summary of the invention
It is an object of the invention to overcome background technique to prepare existing for the method for red schorl phase titanium dioxide nano material
Deficiency, provides that a kind of preparation process is simple, environmental-friendly, synthesis condition is easy to control and low-cost red schorl phase titanium dioxide
The preparation method of nanosphere.
Technical scheme is as follows:
A kind of preparation method of red schorl phase titanium dioxide nano ball, step have:
(1) prepared by Ti electrode: titanium sheet being processed into the electrode slice of coaxial magnetic control plasma accelerator system and device, then through marking
After quasi- Wafer Clean Process cleaning, it is assembled in coaxial magnetic control plasma accelerator system and device, as electric discharge
Cathode serves as the titanium source of reactant；
(2) inflate: after the reaction cavity in coaxial magnetic control plasma accelerator system and device is vacuumized, being filled with purity is
99.7% industrial oxygen stops inflation after system air pressure is restored to 1.5 atmospheric pressure, and the oxygen in cavity serves as reaction
The oxygen source of object；
(3) plasma heating reaction is opened；Make Ti electrode surface that oxidation reaction occur；
(4) it collects product: after reacting ends with system temperature and being cooled to room temperature, valve is opened, from reaction cavity and electricity
Collecting reaction product on pole piece；
(5) anneal: the product that step (4) obtains being transferred in Muffle furnace and is annealed, when after reaction, with furnace from
It is so cooled to room temperature, obtains red schorl phase titanium dioxide nano ball.
A kind of preparation method of red schorl phase titanium dioxide nano ball of the invention, the plasma heating in step (3)
In reaction, the parameter setting of coaxial magnetic control plasma accelerator system is preferred are as follows: charging capacitor 14.4mF, charging voltage are
2.5kV, rechargeable energy 50KJ, discharge power 50Mw, 55 microsecond of pulse duration, a cycle 0.5ms.
A kind of preparation method of red schorl phase titanium dioxide nano ball of the invention, in step (5), annealing temperature is preferred
500~700 DEG C, annealing time preferably 1~6 hour.
The utility model has the advantages that
1, present invention process step is simple and easy, and preparation time is short (0.5ms), and yield is big, and (a cycle 0.5ms can produce
15g), prepare environmental-friendly, at low cost (reaction raw material are cheap and easy to get, only with cheap commercialization titanium sheet and industry oxygen
Gas).
2, nanosphere structural stability prepared by the present invention is good, and crystallinity is high, and product purity is high, and size distribution ranges are narrow,
Particle spherical surface is smooth, and monodispersity is good, can be used for rutile crystalline and the higher field of purity requirement.
Detailed description of the invention
Fig. 1 is device structure schematic diagram used in the embodiment of the present invention 1.
Fig. 2 is scanning electron microscope (SEM) figure of sample obtained by the embodiment of the present invention 2.
Fig. 3 is the raman spectrum of sample obtained by the embodiment of the present invention 2.
Specific embodiment
Following embodiment only for illustration, should not be understood as the limitation to this patent.
1 device structure of embodiment
The structural schematic diagram of preparation system used in the present invention is as shown in Figure 1, its primary structure has in nonmagnetic metal
The coaxial magnetic control plasma that cover 1, plasma generation device 2, nonmagnetic metal outer cover 3, accelerator system 4, ferroelectricity pole piece 6 are constituted
Accelerator system and inductance element system 5, switch 7, capacitor 8, reaction cavity 9.Wherein nonmagnetic metal inner cover 1 and non-magnetic
Property metal casing 3 constitute graphite electrode system, primarily serve heat dissipation and protective effect.The maximum charging voltage of system is 5 kilovolts,
Maximum charge capacitor is 28.8mF.Under the action of plasma generation device 2, the electric current that the electric discharge of capacitor 8 generates converts oxygen
At plasma state, then the accelerated device system 4 of the oxygen of these plasma states accelerate and inductance element system 5 regulate and control exit velocities and
Ferroelectricity pole piece 6 reacts.The reaction temperature of this preparation system can be more than 10000K, and cooling rate is up to 108K/s, plasma add
Rate hasten up to 2.8Km/s.
The preparation of 2 red schorl phase titanium dioxide nano ball of embodiment
(1) prepared by Ti electrode: commercially available high-purity titanium sheet (purity 99.99%) is processed into magnetic control plasma accelerator system
The electrode slice of device, then (deionized water, acetone and absolute alcohol are ultrasonic respectively after the cleaning of standard semiconductor silicon wafer cleaning process
Cleaning is after twenty minutes), it is assembled in the titanium that reactant is served as in the coaxial magnetic control plasma accelerator system and device of embodiment 1
Source.
(2) inflate: after the reaction cavity 9 in the device systems of embodiment 1 is vacuumized, being filled with purity is 99.7% industry
Oxygen stops inflation after system air pressure is restored to 1.5 atmospheric pressure.Oxygen in cavity 9 serves as the oxygen source of reactant.
(3) plasma heating reacts.Equipment reaction parameter setting is as follows: charging capacitor 14.4mF, charging voltage are
2.5kV, rechargeable energy 50KJ, discharge power 50Mw, 55 microsecond of pulse duration, a cycle 0.5ms.
(4) it collects product: after system temperature is cooled to room temperature, valve is opened, from reaction cavity and Ti electrode on piece
Collecting reaction product.One pulse reaction time is 0.5 millisecond, and products therefrom yield is 15g.
(5) it anneals: step (4) products therefrom being transferred in alumina crucible, and is transferred into 600 DEG C of Muffle furnace
It anneals under middle air atmosphere, annealing time is 2 hours.After annealing specimen naturally cools to room temperature with furnace, rutile is obtained
Phase titanium dioxide nano ball product.
As shown in Fig. 2, can be clearly observed grain shape from figure has been the scanning electron microscope (SEM) of the sample of preparation
The spherical shape and surface of beauty are smooth, and the main distribution of partial size is within several nanometers to 500 nanometers, and most of particle sizes are 50
Within nanometer.The raman spectrum of sample is as shown in figure 3, can be determined that the product being prepared is Rutile Type by spectrogram.
Claims (3)
1. a kind of preparation method of red schorl phase titanium dioxide nano ball, step have:
(1) prepared by Ti electrode: titanium sheet being processed into the electrode slice of coaxial magnetic control plasma accelerator system and device, then through standard half
Conductor silicon wafer cleaning process cleaning after, be assembled in coaxial magnetic control plasma accelerator system and device, as electric discharge cathode,
Serve as the titanium source of reactant；The coaxial magnetic control plasma accelerator system and device is by nonmagnetic metal inner cover (1), plasma
Generation device (2), nonmagnetic metal outer cover (3), accelerator system (4), Ti electrode piece (6) are constituted；Described coaxial magnetic control etc.
Ion accelerator arrangement device is also connected with inductance element system (5), switch (7), capacitor (8), reaction cavity (9)；
(2) inflate: after the reaction cavity in coaxial magnetic control plasma accelerator system and device is vacuumized, being filled with purity is
99.7% industrial oxygen stops inflation after system air pressure is restored to 1.5 atmospheric pressure, and the oxygen in cavity serves as reaction
The oxygen source of object；
(3) plasma heating reaction is opened；Under the action of plasma generation device (2), the electric current of capacitor (8) electric discharge generation
Oxygen is converted into plasma state, then the accelerated device system (4) of the oxygen of these plasma states accelerates and inductance element system (5)
Regulation exit velocities are reacted with Ti electrode piece (6), make Ti electrode surface that oxidation reaction occur；
(4) it collects product: after reacting ends with system temperature and being cooled to room temperature, valve is opened, from reaction cavity and electrode slice
Upper collecting reaction product；
(5) it anneals: the product that step (4) obtains being transferred in Muffle furnace and is annealed, it is naturally cold with furnace when after reaction
But to room temperature, red schorl phase titanium dioxide nano ball is obtained.
2. a kind of preparation method of red schorl phase titanium dioxide nano ball according to claim 1, which is characterized in that
In the plasma heating reaction of step (3), the parameter setting of coaxial magnetic control plasma accelerator system are as follows: charging capacitor is
14.4mF, charging voltage 2.5kV, rechargeable energy 50KJ, discharge power 50MW, 55 microsecond of pulse duration, a week
Phase is 0.5ms.
3. a kind of preparation method of red schorl phase titanium dioxide nano ball according to claim 1 or 2, which is characterized in that
In step (5), annealing temperature is 500~700 DEG C, and annealing time is 1~6 hour.
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| CN107988614B (en) * | 2017-10-31 | 2019-05-17 | 华东师范大学 | The preparation method of Grey Reduction type nano titania mixed crystal |
| WO2022249941A1 (en) * | 2021-05-24 | 2022-12-01 | デンカ株式会社 | Inorganic oxide powder, method for producing same, and resin composition |
| EP4349785A1 (en) * | 2021-05-24 | 2024-04-10 | Denka Company Limited | Inorganic oxide powder, method for producing same, and resin composition |
| CN115818709A (en) * | 2022-12-06 | 2023-03-21 | 吉林大学 | Method for controlling dispersity of titanium dioxide |
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Non-Patent Citations (1)
| Title |
|---|
| "Direct Dynamic Synthesis of Nanodispersed Phases of Titanium Oxides upon Sputtering of Electrodischarge Titanium Plasma into an Air Atmosphere";第43卷第1期;《Technical Physics Letters》;20170217;第43卷(第1期);第21-27页 |
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