CN108620057A - A kind of method of electrostatic spinning growth Bi2Ti2O7The preparation method of nano wire - Google Patents

A kind of method of electrostatic spinning growth Bi2Ti2O7The preparation method of nano wire Download PDF

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CN108620057A
CN108620057A CN201810472224.0A CN201810472224A CN108620057A CN 108620057 A CN108620057 A CN 108620057A CN 201810472224 A CN201810472224 A CN 201810472224A CN 108620057 A CN108620057 A CN 108620057A
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electrostatic spinning
solution
nano
nano wire
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葛万银
徐美美
焦思怡
常哲
叶晓慧
张荔
朱建峰
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Shaanxi University of Science and Technology
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Abstract

A kind of method of electrostatic spinning growth Bi2Ti2O7Bismuth nitrate, butyl titanate in acetic acid, ammonium hydroxide are slowly added in reaction system according to certain molar ratio co-dissolve by the preparation method of nano wire, until the acid-base value of whole system is that neutral completion is reacted.It is detached by solution and obtains Bi2Ti2O7Colloid weighs Bi according to a certain percentage2Ti2O7It is dissolved in 10ml ethyl alcohol with PVP and obtains electrostatic spinning precursor liquid, a large amount of nano wires, the Bi obtained after annealed processing can be obtained on the collector by controlling voltage and flow2Ti2O7Nano-powder has efficient Photocatalytic Degradation Property, has very high degradation rate especially for rhdamine B molecule.Under ultraviolet light to the degradation rate of rhodamine B, 90% or more can be reached in 30 minutes.Used method can obtain the Bi of pure phase2Ti2O7Nano-powder, this method is simple and practicable, reproducible.Acid-base value when entire reaction system reaction is completed is neutrality, to environment without any pollution.

Description

A kind of method of electrostatic spinning growth Bi2Ti2O7The preparation method of nano wire
Technical field
The present invention relates to inorganic ternary Bi2Ti2O7Prepared by compound nano-material and efficient photochemical catalyst researches and develops field, Bi is grown more particularly to a kind of method of electrostatic spinning2Ti2O7The preparation method of nano wire.
Background technology
Bi2Ti2O7Ternary compound is cubic pyrochlore structure, belongs to Fd-3m (227) space group, lattice constant isa= 10.2331 angstroms.Bi-Ti-O ternary compounds include such as Bi4Ti3O12, Bi2Ti4O11, Bi12TiO20, Bi8TiO14Equal chemical combination Object.It is relatively narrow that Henderson etc. once reports band gap, has absorption in visible light, has visible light catalysis activity（Henderso S J, Shebanova O, Hector A L, et al., Structural Variations in Pyrochlore- Structured Bi2Hf2O7, Bi2Ti2O7 and Bi2Hf2-xTixO7 Solid Solutions as a Function of Composition and Temperature by Neutron and X-ray Diffraction and Raman Spectroscopy [J], Chem.Mater., 2007,19 (7):1712-1722）；In addition, it can also act as insulated gate field effect Should pipe grid material to improve the mutual conductance of isolated gate FET, reduce cut-in voltage, improve resistance to breakdown characteristics, reduce device Size reduces cost etc.（Xiao Zhuo Ping, Wu Xianming, Wang Shaowei wait film preparations and insulated-gate field-effect Pipe development ［ J ］ functional materials and device journal, 2001,7 (2): 171-174）；In addition, it is also used as PZT ferroelectricities The buffer layer of film plays the role of improving Electrical property（Wang S W, Wang H, Shang S X, et al. PZT thin films pre-pared by chemical solution decomposition using a Bi2Ti2O7 Buffer layer ［ J ］ J. Crystal Growth, 2000,217 (11): 388-392）.It can be seen that Bi2Ti2O7 Ternary compound not only has learning value, but also has practical value.For this purpose, preparing and studying ternary compound Bi2Ti2O7Nano material seems extremely important.Patent of invention CN201510393909.2 is reported, by Bi (NO3)3With acetic anhydride Be completely dissolved to obtain solution 1, then butyl titanate is dissolved in ethylene glycol adds glacial acetic acid and obtain solution 2, then by solution 1 with Solution 2 mixes, and is put into oven drying, then calcines, keeps the temperature, is cooling to obtain a nanometer Bi2Ti2O7Powder.Patent of invention CN201310453437.6 report hydro-thermal method synthesis Bismuth titanate nanoneedle method, but the bismuth titanates obtained by cube Bi2Ti2O7 and Bi12TiO20 crystalline phases are constituted.Bi2Ti2O7One-dimensional nano line is due to big specific surface area and special one-dimensional knot Structure had both met the required bigger serface of photocatalysis, also meets photo-generate electron-hole to being transmitted along one-dimensional square, avoids Photo-generated carrier it is compound, be conducive to obtain outstanding photocatalysis performance.For this purpose, research obtains one-dimensional Bi2Ti2O7Nano wire Technique seem especially important.Prepare Bi2Ti2O7The technological difficulties of nano material are, the accurate control for its chemical composition System, obtain have theoretical stoichiometric than ternary compound.Bismuth element and titanium elements are when forming compound, it is easier to Form ternary BiTiO3(orthorhombic phase) and Bi3Ti4O12(monoclinic phase) compound causes to be formed by product, often contains others Dephasign.In order to obtain Bi2Ti2O7Monodimension nanometer material, the shortcomings that overcoming prior art route, this patent is intended to accurately control Stoichiometric ratio between ternary Bi-Ti-O chemical elements, to obtain pure phase Bi2Ti2O7, while the method for passing through electrostatic spinning Obtain one-dimensional nano wire predecessor.Pure cubic phase is obtained by subsequent heat treatment, and photocatalytic activity obtains pole Big raising.
Invention content
In order to overcome above-mentioned existing defect existing in the prior art, the object of the present invention is to provide a kind of method of electrostatic spinning Grow Bi2Ti2O7The preparation method of nano wire is solvent using DMF, and appropriate PVP is added, and passes through heating, heat preservation and cooling Three phases grow pure Bi2Ti2O7Nano material.
In order to achieve the above object, the present invention adopts the following technical scheme that：
A kind of method of electrostatic spinning growth Bi2Ti2O7The preparation method of nano wire, includes the following steps：
1）According to（1~1.3）：Bismuth nitrate and butyl titanate are mixed to be dispersed in 10ml acetic acid by 1 molar ratio obtains solution A；
2）Under rapid stirring, ammonium hydroxide is added in solution A rapidly, adjusts the ph values of solution to neutrality, by molten Liquid separation obtains colloid B；
3）Colloid B is put into electric drying oven with forced convection dry；
4）Colloid B after drying is dispersed in the DMF solution added with appropriate PVP, electrostatic spinning precursor liquid is made into；
5）In the case where application voltage is the high voltage power supply under the conditions of 10-25KV flows are 25 μm/m, precursor liquid is passed through micro- Amount flow precession device is ejected on collector;.
6）After waiting for electrostatic spinning, the nano wire on collector is transferred in Muffle furnace and with the speed of 2.5 DEG C/min Rate is raised to 500 DEG C and keeps the temperature 1 hour, you can obtains the pure phase Bi that crystal property is high, photocatalysis performance is good2Ti2O7Nano material;
7）By the high pure phase Bi of the crystal property of acquisition2Ti2O7Nano material carries out the photocatalytic degradation analysis of organic dyestuff, card It is real that there is particularly preferred decomposition degradation effect to rhodamine.
Solution separation method in the step 2) includes filtering or centrifugation purification.
The molar ratio that colloid B is dispersed in PVP in the step 4) is 2：5.
The step 5）In micro flow precession device rate be 15-70 μm/m.
It is in simulated solar irradiation as light source to the experiment of rhodamine photocatalytic degradation in the step six.
Compared with prior art, the present invention has technique effect beneficial below：
Using DMF as solvent in the present invention, the high pure phase Bi of crystal property is prepared using the method for electrostatic spinning2Ti2O7Nanometer material Material.Compared with other methods for preparing nano material, the method for electrostatic spinning has the characteristics that operation is easy and efficient, and can The problems such as to avoid disperseing caused by distribution of particles is uneven, reuniting.
Further, appropriate PVP is added when configuring precursor liquid in the present invention, and cost is very cheap, and has to environment without any Evil substance.Bismuth nitrate/PVP molal weights ratio most preferably 2：5, taylor cone appearance is at this time had in spinning process.
Description of the drawings
Fig. 1 is the Bi of the present invention2Ti2O7Fiber pictorial diagram；
Fig. 2 is the Bi that the present invention is grown2Ti2O7The X-ray diffractogram of powder；
Fig. 3 is the Bi that the present invention is obtained2Ti2O7Absorption spectra of the nano-powder after different time degrades to rhodamine；
Fig. 4 is the present invention under ultraviolet light using proportioning Bi:Ti:O is 2：2：7 Bi grown2Ti2O7Nano material with not Bi through electrostatic spinning2Ti2O7Nano material degrade under the same conditions rhodamine photocatalytic activity comparison diagram；
Fig. 5 is the X-ray diffractogram of example 2；
Fig. 6 is the X-ray diffractogram of example 3；
Fig. 7 is the X-ray diffractogram of example 4；
Fig. 8 is the X-ray diffractogram of example 5.
Specific implementation mode
Method of electrostatic spinning prepares Bi2Ti2O7Nano material is related to following process.First, raw material and acetic acid are put into In ultrasonic instrument.Then, pass through oscillation so that reaction raw materials fully dissolve.In continuous oscillatory process, four fourth of metatitanic acid is added Ammonium hydroxide is then added in ester, you can obtains solution A.Solution A is centrifuged, colloid B can be obtained.Colloid B dispersions after drying In the DMF solution added with appropriate PVP, it is made into electrostatic spinning precursor liquid.In the case where applying high voltage power supply, precursor liquid is led to Micro flow precession device is crossed to be ejected on collector.After waiting for electrostatic spinning, the nano wire on collector is carried out at annealing Reason obtains the high pure phase Bi of crystal property2Ti2O7Nano material.
The present invention specifically includes following steps：
A kind of method of electrostatic spinning growth Bi2Ti2O7The preparation method of nano wire, includes the following steps：
1）According to（1~1.3）：Bismuth nitrate and butyl titanate are mixed to be dispersed in 10ml acetic acid by 1 molar ratio obtains solution A；
2）Under rapid stirring, ammonium hydroxide is added in solution A rapidly, adjusts the ph values of solution to neutrality, by molten Liquid separation obtains colloid B；
3）Colloid B is put into electric drying oven with forced convection dry；
4）Colloid B after drying is dispersed in the DMF solution added with appropriate PVP, electrostatic spinning precursor liquid is made into；
5）In the case where application voltage is the high voltage power supply under the conditions of 10-25KV flows are 25 μm/m, precursor liquid is passed through micro- Amount flow precession device is ejected on collector;.
6）After waiting for electrostatic spinning, the nano wire on collector is transferred in Muffle furnace and with the speed of 2.5 DEG C/min Rate is raised to 500 DEG C and keeps the temperature 1 hour, you can obtains the pure phase Bi that crystal property is high, photocatalysis performance is good2Ti2O7Nano material;
7）By the high pure phase Bi of the crystal property of acquisition2Ti2O7Nano material carries out the photocatalytic degradation analysis of organic dyestuff, card It is real that there is particularly preferred decomposition degradation effect to rhodamine.
The solution acid alkalinity of produced mistake is in neutrality in the present invention, is not involved in the problems, such as any subsequent wastewater treatment, to ring Border does not have any harm, is a kind of simple and green synthesis technology.
Embodiment 1
By bismuth nitrate, butyl titanate according to 1:1.2 molar ratio co-dissolve passes through supersound process in 10 milliliters of acetic acid Form transparent solution；The temperature for adjusting water-bath is 10 DEG C, ammonium hydroxide is slowly added in transparent solution, and breast is generated in solution White product continues to add ammonium hydroxide until the acid-base value of whole system is neutrality, completion reaction.It is detached and is obtained by solution Bi2Ti2O7Colloid.Then Bi is weighed2Ti2O7 0.61g is dispersed in 10ml ethanol solutions, the PVP of 0.39g is then added, through magnetic Electrostatic spinning precursor liquid is obtained after power stirring, is that 15KV goes out on the collector under conditions of flow is 25 μm/m in control voltage After waiting for electrostatic spinning, the nano wire on collector is transferred in Muffle furnace and with 2.5 DEG C/min's for now a large amount of nano wires Rate is raised to 500 DEG C and keeps the temperature 1 hour, you can obtains the pure phase Bi that crystal property is high, photocatalysis performance is good2Ti2O7Nano material.
As shown in Fig. 2, the powder obtained is scanned using X-ray diffractometer between 10-80 degree, powder sample is aobvious Polycrystalline diffraction characteristics, all diffraction maximums and Bi are shown2Ti2O7Standard card (PDF#97-016-1101) fits like a glove, and does not have Any miscellaneous peak occurs, it was demonstrated that the powder obtained is Bi2Ti2O7Pure phase.Wherein 2 θ angles are highest peaks at 29.91 °, corresponding Bi2Ti2O7(222) crystal face of standard card.
Embodiment 2
By bismuth nitrate, butyl titanate according to 1:1.1 molar ratio co-dissolve is in 10 milliliters of acetic acid, sonicated shape At transparent solution；Ammonium hydroxide is slowly added in transparent solution, milky white product is generated in solution, it is straight to continue addition ammonium hydroxide Acid-base value to whole system is neutrality, completes reaction.It is detached by solution and obtains Bi2Ti2O7Colloid.Then it weighs Bi2Ti2O7 0.49g is dispersed in 10ml ethanol solutions, and 0.50 PVP is then added, electrostatic spinning is obtained after magnetic agitation Precursor liquid is that 15KV a large amount of nano wires occurs, wait for electrostatic on the collector under conditions of flow is 25 μm/m in control voltage After spinning, the nano wire on collector is transferred in Muffle furnace and 500 DEG C of heat preservations 1 are raised to the rate of 2.5 DEG C/min Hour, you can obtain the pure phase Bi that crystal property is high, photocatalysis performance is good2Ti2O7Nano material.
Its X-ray diffractogram is as shown in Figure 5：
Embodiment 3
By bismuth nitrate, butyl titanate according to 1:1.3 molar ratio co-dissolve is in 10 milliliters of acetic acid, sonicated shape At transparent solution；Ammonium hydroxide is slowly added in transparent solution, milky white product is generated in solution, it is straight to continue addition ammonium hydroxide Acid-base value to whole system is neutrality, completes reaction.It is detached by solution and obtains Bi2Ti2O7Colloid.Then it weighs Bi2Ti2O7 0.32g is dispersed in 10ml ethanol solutions, and the PVP of 1.82g is then added, electrostatic spinning is obtained after magnetic agitation Precursor liquid is that 19.67KV a large amount of nano wires occurs, wait for quiet on the collector under conditions of flow is 70 μm/m in control voltage After Electrospun, the nano wire on collector is transferred in Muffle furnace and 500 DEG C of heat preservations are raised to the rate of 2.5 DEG C/min 1 hour, you can obtain the pure phase Bi that crystal property is high, photocatalysis performance is good2Ti2O7Nano material.
Its X-ray diffractogram is as shown in Figure 6：
Embodiment 4
By bismuth nitrate, butyl titanate according to 1:1.15 molar ratio co-dissolve is in 10 milliliters of acetic acid, sonicated shape At transparent solution；Ammonium hydroxide is slowly added in transparent solution, milky white product is generated in solution, it is straight to continue addition ammonium hydroxide Acid-base value to whole system is neutrality, completes reaction.It is detached by solution and obtains Bi2Ti2O7Colloid.Then it weighs Bi2Ti2O7 1.00g is dispersed in 10ml ethanol solutions, and the PVP of 0.33g is then added, electrostatic spinning is obtained after magnetic agitation Precursor liquid is that 15.00KV a large amount of nano wires occurs, wait for quiet on the collector under conditions of flow is 15 μm/m in control voltage After Electrospun, the nano wire on collector is transferred in Muffle furnace and 500 DEG C of heat preservations are raised to the rate of 0.5 DEG C/min 1 hour, you can obtain the pure phase Bi that crystal property is high, photocatalysis performance is good2Ti2O7Nano material.
Its X-ray diffractogram is as shown in Figure 7：
Embodiment 5
By bismuth nitrate, butyl titanate according to 1:1.25 molar ratio co-dissolve is in 10 milliliters of acetic acid, sonicated shape At transparent solution；Ammonium hydroxide is slowly added in transparent solution, milky white product is generated in solution, it is straight to continue addition ammonium hydroxide Acid-base value to whole system is neutrality, completes reaction.It is detached by solution and obtains Bi2Ti2O7Colloid.Then it weighs Bi2Ti2O7 1.00g is dispersed in 10ml ethanol solutions, and the PVP of 0.33g is then added, electrostatic spinning is obtained after magnetic agitation Precursor liquid is that 15.00KV a large amount of nano wires occurs, wait for quiet on the collector under conditions of flow is 15 μm/m in control voltage After Electrospun, by the nano wire on collector in N2Atmosphere under, be heated slowly to 500 DEG C, you can obtain crystal property Bi high, photocatalysis performance is good2Ti2O7Nano material.Its X-ray diffractogram is as shown in Figure 8.

Claims (5)

1. a kind of method of electrostatic spinning grows Bi2Ti2O7The preparation method of nano wire, which is characterized in that include the following steps：
1）According to（1~1.3）：Bismuth nitrate and butyl titanate are mixed to be dispersed in 10ml acetic acid by 1 molar ratio obtains solution A；
2）Under rapid stirring, ammonium hydroxide is added in solution A rapidly, adjusts the ph values of solution to neutrality, ph can be used Meter is monitored in real time, is detached by solution and is obtained colloid B；
3）Colloid B is put into electric drying oven with forced convection dry；
4）Colloid B after drying is dispersed in the DMF solution added with appropriate PVP, electrostatic spinning precursor liquid is made into；
5）In the case where application voltage is the high voltage power supply under the conditions of 10-25KV flows are 25 μm/m, precursor liquid is passed through micro- Amount flow precession device is ejected on collector；
6）After waiting for electrostatic spinning, the nano wire on collector is transferred in Muffle furnace and with the rate liter of 2.5 DEG C/min 1 hour is kept the temperature to 500 DEG C, you can obtains the pure phase Bi that crystal property is high, photocatalysis performance is good2Ti2O7Nano material;
7）By the high pure phase Bi of the crystal property of acquisition2Ti2O7Nano material carries out the photocatalytic degradation analysis of organic dyestuff, card It is real that there is particularly preferred decomposition degradation effect to rhodamine.
2. a kind of method of electrostatic spinning according to claim 1 grows Bi2Ti2O7The preparation method of nano wire, feature exist In the solution separation method in the step 2) includes filtering or centrifugation purification.
3. a kind of method of electrostatic spinning according to claim 1 grows Bi2Ti2O7The preparation method of nano wire, feature exist In the molar ratio that colloid B is dispersed in PVP in the step 4) is 2：5.
4. a kind of method of electrostatic spinning according to claim 1 grows Bi2Ti2O7The preparation method of nano wire, feature exist In the step 5）In micro flow precession device rate be 15-70 μm/m.
5. a kind of method of electrostatic spinning according to claim 1 grows Bi2Ti2O7The preparation method of nano wire, feature exist In being in simulated solar irradiation as light source to the experiment of rhodamine photocatalytic degradation in the step six.
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CN114456622A (en) * 2022-02-14 2022-05-10 费县三鼎工程科技中心 Coating with formaldehyde purification and antibacterial functions

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CN109371502A (en) * 2018-11-15 2019-02-22 陕西科技大学 A kind of cubic pyrochlore phase nanofiber preparation method and applications based on method of electrostatic spinning
CN109913979A (en) * 2019-03-15 2019-06-21 陕西科技大学 A kind of holmium double doped miscellaneous Jiao Lvshi phase nanofiber preparation method and applications of rare earth ytterbium
CN109943915A (en) * 2019-03-15 2019-06-28 陕西科技大学 A kind of ytterbium thulium codope blue-light-emitting Jiao Lvshi phase nanofiber preparation method and applications
CN109943916A (en) * 2019-03-15 2019-06-28 陕西科技大学 A kind of rare earth ytterbium erbium codope Jiao Lvshi phase nanofiber preparation method and applications
CN109913979B (en) * 2019-03-15 2022-02-01 陕西科技大学 Preparation method and application of rare earth ytterbium and holmium double-doped pyrochlore phase nanofiber
CN109943915B (en) * 2019-03-15 2022-02-01 陕西科技大学 Preparation method and application of ytterbium and thulium double-doped blue luminescent pyrochlore phase nanofiber
CN109943916B (en) * 2019-03-15 2022-02-01 陕西科技大学 Preparation method and application of rare earth ytterbium and erbium co-doped pyrochlore phase nanofiber
CN114456622A (en) * 2022-02-14 2022-05-10 费县三鼎工程科技中心 Coating with formaldehyde purification and antibacterial functions
CN114456622B (en) * 2022-02-14 2022-09-23 山西亮龙涂料有限公司 Coating with formaldehyde purification and antibacterial functions

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