CN102275986A - Controllable hydro-thermal preparation method for titanium dioxide nanobelts of different crystal forms - Google Patents
Controllable hydro-thermal preparation method for titanium dioxide nanobelts of different crystal forms Download PDFInfo
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Abstract
The invention discloses a controllable dydro-thermal preparation method for titanium dioxide nanobelts of different crystal forms, belonging to the technical field of preparation of nanometer materials. The method comprises the following steps of: dispersing TiO2 nanometer powder into a NaOH aqueous solution and undergoing a hydro-thermal reaction at the temperature of 170-190 DEG C; putting an obtained white product into a HCl solution for performing ion exchange, washing away excessive hydrochloric acid with deionized water, and drying to obtain hydrogen-titanium acid; and calcining the hydrogen-titanium acid at the temperature of 400 DEG C to obtain TiO2 nanobelts. By controlling the amount of the TiO2 nanometer powder dispersed in the NaOH solution, final products are controlled to be pure anatase phase, anatase, TiO2-B mixed crystal and pure TiO2-B-phase TiO2 nanobelts. By merely adjusting the adding quantity of a reactant, the aim of adjusting the appearance and crystal form of the product is fulfilled; the method has the advantages of simple process, high controllability, low cost and environmental friendliness; and the prepared product can be applied by serving as photocatalysis materials and lithium battery electrode materials.
Description
Technical field
The present invention relates to the technical field of nano material preparation, what be specifically related to is with the get everything ready novel method of titanium dioxide nano-belts of different crystal forms of hydrothermal method may command.
Background technology
Titanium dioxide (TiO
2) be a kind of important semiconductor material with wide forbidden band, have that stability is high, nontoxic, biologically stable is good, characteristics such as uv-absorbing have wide application prospect in fields such as environment, information, material, the energy, medical and health.In recent years, along with developing rapidly of nanotechnology, TiO
2Nano material embodies many character that is better than other material, makes TiO
2There is wide application prospect in nano material at aspects such as new function material and nano-devices.Therefore, the TiO of different-shape and crystal formation
2Nano material be prepared into focus for people research.
In early days, TiO
2The preparation research of nano material mainly concentrates on the nano particle, utilizes chemical processes such as sol-gel, can obtain the TiO of anatase octahedrite and rutile-type by calcination processing
2Nano particle.In recent years, utilize the hydrothermal method people successfully to prepare anatase octahedrite phase TiO again
2Nanotube and TiO
2-B nano belt.But, for different-shape and crystal formation TiO
2The research of the controlled preparation of nano material also lacks systematic account.At TiO
2Have been found that in the research of character such as the photochemical catalysis of nano material that the nano material with mixed crystal type often embodies more excellent physics-chem characteristic.Yet the TiO of synthetic pure phase still mainly is devoted in existing research
2Nano material does not also prepare different-shape and crystal formation TiO about the amount of filling by reactant in the adjusting hydrothermal reaction so far
2The report of nano material.
Summary of the invention
Purpose of the present invention prepares different crystal forms TiO with regard to providing a kind of amount of filling by reactant in the adjusting hydrothermal reaction
2The novel method of nano belt.
Involved in the present invention is with titanic oxide nano and sodium hydroxide is raw material, utilizes hydro-thermal reaction to prepare different crystal forms TiO
2The method of nano belt.The steps include: a certain amount of reactant TiO
2The sodium hydroxide that nano powder is scattered in high density (in 9～11mol/L) aqueous solution, fully stirs 20～30min.The gained suspension liquid is transferred in the hydrothermal reaction kettle, and under differential responses thing addition (0.2,0.5,0.8,1,2,3,4,5 and 6g) condition, 170～190 ℃ are carried out hydro-thermal reaction 65～75h respectively.Gained hydro-thermal reaction gained white product placed (0.1～1mol/L) dilute hydrochloric acid solution floods 8～12h, carries out sufficient ion-exchange.By suction filtration,, with the products therefrom oven dry, obtain intermediate product (hydrogen metatitanic acid) again with the excessive hydrochloric acid of deionized water flush away.Gained hydrogen metatitanic acid is kept 400 ℃ of calcinings of temperature 4h in tube furnace, obtain pure anatase octahedrite phase, anatase octahedrite and TiO
2-B mixed crystal and pure TiO
2The TiO of-B phase
2Nano belt.
The concrete TiO for preparing pure anatase octahedrite phase that is divided into
2Nano belt, anatase octahedrite phase and TiO
2The mixed crystal type TiO of-B phase
2Nano belt, TiO
2The TiO of-B phase
2Three technical schemes of nano belt, each technical scheme is as follows.
A kind of controlled hydrothermal preparing process of different crystal forms titanium dioxide nano-belts is 0.2～0.6: 4.8 TiO with mass ratio
2Nano powder and NaOH are raw material; With TiO
2Nano powder is scattered in the NaOH aqueous solution, stirs 20～30min, and the suspension liquid that obtains is transferred in the hydrothermal reaction kettle, carries out hydro-thermal reaction 65～75h under 170～190 ℃, obtains white product; Place HCl solution to flood 8～12h white product, carry out ion-exchange, suction filtration, with the excessive hydrochloric acid of deionized water flush away, oven dry obtains the intermediate hydrogen metatitanic acid again; The hydrogen metatitanic acid at 400 ℃ of calcinings of temperature 4h, is obtained the TiO of pure anatase octahedrite phase
2Nano belt.
A kind of controlled hydrothermal preparing process of different crystal forms titanium dioxide nano-belts is 0.8～4: 4.8 TiO with mass ratio
2Nano powder and NaOH are raw material; With TiO
2Nano powder is scattered in the NaOH aqueous solution, stirs 20～30min, and the suspension liquid that obtains is transferred in the hydrothermal reaction kettle, carries out hydro-thermal reaction 65～75h under 170～190 ℃, obtains white product; Place HCl solution to flood 8～12h white product, carry out ion-exchange, suction filtration, with the excessive hydrochloric acid of deionized water flush away, oven dry obtains the intermediate hydrogen metatitanic acid again; The hydrogen metatitanic acid is kept 400 ℃ of calcinings of temperature 4h in tube furnace, obtain anatase octahedrite phase and TiO
2The mixed crystal type TiO of-B phase
2Nano belt.
A kind of controlled hydrothermal preparing process of different crystal forms titanium dioxide nano-belts is 5～6: 4.8 TiO with mass ratio
2Nano powder and NaOH are raw material; With TiO
2Nano powder is scattered in the NaOH aqueous solution, stirs 20～30min, and the suspension liquid that obtains is transferred in the hydrothermal reaction kettle, carries out hydro-thermal reaction 65～75h under 170～190 ℃, obtains white product; Place HCl solution to flood 8～12h white product, carry out ion-exchange, suction filtration, with the excessive hydrochloric acid of deionized water flush away, oven dry obtains the intermediate hydrogen metatitanic acid again; The hydrogen metatitanic acid is kept 400 ℃ of calcinings of temperature 4h in tube furnace, obtain TiO
2The TiO of-B phase
2Nano belt.
In three above-mentioned technical schemes, described sodium hydroxide solution, concentration is 9～11mol/L; Described hydrochloric acid soln, concentration are 0.1～1mol/L.
The beneficial effect that method of the present invention and background technology relatively have is as follows: by conditioned reaction thing (TiO
2Powder) addition has been realized the purpose of regulation and control product pattern and crystal formation, has obtained pure anatase octahedrite phase, anatase octahedrite and TiO respectively
2-B mixed crystal and pure TiO
2The TiO of-B phase
2Nano belt.Hydrothermal Preparation TiO in the past
2In the process of nano material, obtain the TiO of anatase octahedrite phase often by conditioned reaction temperature or reaction times
2Nanotube or TiO
2The nano belt of-B phase, but be difficult to obtain the mixed crystal type TiO of the nano belt and the adjustable ratio of anatase octahedrite phase
2Nano belt.And the present invention is under conditions such as fixation reaction temperature and reaction times, by single conditioned reaction thing (TiO
2Powder) addition has successfully been realized the purpose of regulation and control product pattern and crystal formation.Method technology of the present invention is simple, controllability is strong, with low cost, environmental friendliness, and the product that makes will be applied as photocatalyst material, electrode material of lithium battery.
Description of drawings
Fig. 1 is the TiO of the pure anatase octahedrite phase that makes of embodiment 1
2Nano belt Electronic Speculum photo.
Fig. 2 is the TiO of the pure anatase octahedrite phase that makes of embodiment 1
2Nano belt x ray diffraction spectrogram.
Fig. 3 is the TiO of the pure anatase octahedrite phase that makes of embodiment 2
2Nano belt Electronic Speculum photo.
Fig. 4 is the TiO of the pure anatase octahedrite phase that makes of embodiment 2
2Nano belt x ray diffraction spectrogram.
Fig. 5 be embodiment 3 make contain trace Ti O
2The nano belt Electronic Speculum photo of-B phase.
Fig. 6 be embodiment 3 make contain trace Ti O
2The TiO of-B phase
2Nano belt x ray diffraction spectrogram.
Fig. 7 be embodiment 4 make contain a small amount of TiO
2The TiO of-B phase
2Nano belt Electronic Speculum photo.
Fig. 8 be embodiment 4 make contain a small amount of TiO
2The TiO2 nano belt x ray diffraction spectrogram of-B phase.
Fig. 9 is anatase octahedrite phase and the TiO that embodiment 5 makes
2The mixed crystal type TiO of-B phase
2Nano belt Electronic Speculum photo.
Figure 10 is anatase octahedrite phase and the TiO that embodiment 5 makes
2The mixed crystal type TiO of-B phase
2Nano belt x ray diffraction spectrogram.
Figure 11 is anatase octahedrite phase and the TiO that embodiment 6 makes
2The mixed crystal type TiO of-B phase
2Nano belt Electronic Speculum photo.
Figure 12 is anatase octahedrite phase and the TiO that embodiment 6 makes
2The mixed crystal type TiO of-B phase
2Nano belt x ray diffraction spectrogram.
Figure 13 is anatase octahedrite phase and the TiO that embodiment 7 makes
2The mixed crystal type TiO of-B phase
2Nano belt Electronic Speculum photo.
Figure 14 is anatase octahedrite phase and the TiO that embodiment 7 makes
2The mixed crystal type TiO of-B phase
2Nano belt x ray diffraction spectrogram.
Figure 15 is the pure TiO that embodiment 8 makes
2-B phase TiO
2Nano belt Electronic Speculum photo.
Figure 16 is the pure TiO that embodiment 8 makes
2-B phase TiO
2Nano belt x ray diffraction spectrogram.
Figure 17 is the pure TiO that embodiment 9 makes
2The TiO of-B phase
2Nano belt Electronic Speculum photo.
Figure 18 is the pure TiO that embodiment 9 makes
2The TiO of-B phase
2Nano belt x ray diffraction spectrogram.
Embodiment
Further set forth the present invention below in conjunction with specific embodiment.
Embodiment 1:
It is in the 10mol/L sodium hydroxide solution that 0.2g titanic oxide nano (P25) is scattered in 12 ml concns, place beaker fully to stir 30min, the gained suspension liquid is transferred in the hydrothermal reaction kettle (14 milliliters of volumes) of polytetrafluoroethylliner liner, reactor is placed thermostat container, keep temperature to carry out hydro-thermal reaction 72h for 180 ℃.Hydro-thermal reaction gained white product moved in the dilute hydrochloric acid solution that concentration is 0.5mol/L flood 8h, carry out sufficient ion-exchange.By suction filtration, with deionized water flush away excessive hydrochloric acid, again with products therefrom 80 ℃ of oven dry, obtain intermediate product (hydrogen metatitanic acid).Gained hydrogen metatitanic acid is kept 400 ℃ of calcinings of temperature 4h in tube furnace, obtain the TiO of pure anatase octahedrite phase
2Nano belt, nano belt width are 600～1800nm, and length is 5～15 microns.
Conclusion: when adding 0.2g titanic oxide nano (P25), can prepare the TiO of pure anatase octahedrite phase
2Nano belt, nano belt width are 600～1800nm, and length is 5～20 microns.
Embodiment 2:
It is in the 10mol/L sodium hydroxide solution that 0.5g titanic oxide nano (P25) is scattered in 12 ml concns, place beaker fully to stir 30min, the gained suspension liquid is transferred in the hydrothermal reaction kettle (14 milliliters of volumes) of polytetrafluoroethylliner liner, reactor is placed thermostat container, keep temperature to carry out hydro-thermal reaction 72h for 180 ℃.Hydro-thermal reaction gained white product moved in the dilute hydrochloric acid solution that concentration is 0.5mol/L flood 8h, carry out sufficient ion-exchange.By suction filtration, with deionized water flush away excessive hydrochloric acid, again with products therefrom 80 ℃ of oven dry, obtain intermediate product (hydrogen metatitanic acid).Gained hydrogen metatitanic acid is kept 400 ℃ of calcinings of temperature 4h in tube furnace, obtain the TiO of pure anatase octahedrite phase
2Nano belt, nano belt width are 400～2200nm, and length is 5～20 microns.
Conclusion: when adding 0.5g titanic oxide nano (P25), can prepare the TiO of pure anatase octahedrite phase
2Nano belt, nano belt width are 400～2200nm, and length is 4～15 microns.
Embodiment 3:
It is in the 10mol/L sodium hydroxide solution that 0.8g titanic oxide nano (P25) is scattered in 12 ml concns, place beaker fully to stir 30min, the gained suspension liquid is transferred in the hydrothermal reaction kettle (14 milliliters of volumes) of polytetrafluoroethylliner liner, reactor is placed thermostat container, keep temperature to carry out hydro-thermal reaction 72h for 180 ℃.Hydro-thermal reaction gained white product moved in the dilute hydrochloric acid solution that concentration is 0.5mol/L flood 8h, carry out sufficient ion-exchange.By suction filtration, with deionized water flush away excessive hydrochloric acid, again with products therefrom 80 ℃ of oven dry, obtain intermediate product (hydrogen metatitanic acid).Gained hydrogen metatitanic acid is kept 400 ℃ of calcinings of temperature 4h in tube furnace, obtaining anatase octahedrite is the main trace Ti O that contains mutually
2The TiO of-B phase
2Nano belt, nano belt width are 100～200nm, and length is 2～15 microns.
Conclusion: when adding 0.8g titanic oxide nano (P25), can prepare anatase octahedrite is the main trace Ti O that contains mutually
2The TiO of-B phase
2Nano belt, nano belt width are 100～200nm, and length is 2～15 microns.
Embodiment 4:
It is in the 10mol/L sodium hydroxide solution that 1.0g titanic oxide nano (P25) is scattered in 12 ml concns, place beaker fully to stir 30min, the gained suspension liquid is transferred in the hydrothermal reaction kettle (14 milliliters of volumes) of polytetrafluoroethylliner liner, reactor is placed thermostat container, keep temperature to carry out hydro-thermal reaction 72h for 180 ℃.Hydro-thermal reaction gained white product moved in the dilute hydrochloric acid solution that concentration is 0.5mol/L flood 8h, carry out sufficient ion-exchange.By suction filtration, with deionized water flush away excessive hydrochloric acid, again with products therefrom 80 ℃ of oven dry, obtain intermediate product (hydrogen metatitanic acid).Gained hydrogen metatitanic acid is kept 400 ℃ of calcinings of temperature 4h in tube furnace, obtaining anatase octahedrite is main a small amount of TiO that contains mutually
2The TiO of-B phase
2Nano belt, nano belt width are 50～200nm, and length is 2～15 microns.
Conclusion: when adding 1.0g titanic oxide nano (P25), can prepare anatase octahedrite is main a small amount of TiO that contains mutually
2The TiO of-B phase
2Nano belt, nano belt width are 50～200nm, and length is 2～15 microns.
Embodiment 5:
It is in the 10mol/L sodium hydroxide solution that 2.0g titanic oxide nano (P25) is scattered in 12 ml concns, place beaker fully to stir 30min, the gained suspension liquid is transferred in the hydrothermal reaction kettle (14 milliliters of volumes) of polytetrafluoroethylliner liner, reactor is placed thermostat container, keep temperature to carry out hydro-thermal reaction 72h for 180 ℃.Hydro-thermal reaction gained white product moved in the dilute hydrochloric acid solution that concentration is 0.5mol/L flood 8h, carry out sufficient ion-exchange.By suction filtration, with deionized water flush away excessive hydrochloric acid, again with products therefrom 80 ℃ of oven dry, obtain intermediate product (hydrogen metatitanic acid).Gained hydrogen metatitanic acid is kept 400 ℃ of calcinings of temperature 4h in tube furnace, obtain anatase octahedrite phase and TiO
2The mixed crystal type TiO of-B phase
2Nano belt, nano belt width are 50～200nm, and length is 2～15 microns.
Conclusion: when adding 2.0g titanic oxide nano (P25), can prepare anatase octahedrite phase and TiO
2The mixed crystal type TiO of-B phase
2Nano belt, nano belt width are 50～200nm, and length is 2～15 microns.
Embodiment 6:
It is in the 10mol/L sodium hydroxide solution that 3.0g titanic oxide nano (P25) is scattered in 12 ml concns, place beaker fully to stir 30min, the gained suspension liquid is transferred in the hydrothermal reaction kettle (14 milliliters of volumes) of polytetrafluoroethylliner liner, reactor is placed thermostat container, keep temperature to carry out hydro-thermal reaction 72h for 180 ℃.Hydro-thermal reaction gained white product moved in the dilute hydrochloric acid solution that concentration is 0.5mol/L flood 8h, carry out sufficient ion-exchange.By suction filtration, with deionized water flush away excessive hydrochloric acid, again with products therefrom 80 ℃ of oven dry, obtain intermediate product (hydrogen metatitanic acid).Gained hydrogen metatitanic acid is kept temperature 400 calcining 4h in tube furnace, obtain anatase octahedrite phase and TiO
2The mixed crystal type TiO of-B phase
2Nano belt, nano belt width are 50～200nm, and length is 2～15 microns.
Conclusion: when adding 3.0g titanic oxide nano (P25), can prepare anatase octahedrite phase and TiO
2The mixed crystal type TiO of-B phase
2Nano belt, nano belt width are 50～200nm, and length is 2～15 microns.
Embodiment 7:
It is in the 10mol/L sodium hydroxide solution that 4.0g titanic oxide nano (P25) is scattered in 12 ml concns, place beaker fully to stir 30min, the gained suspension liquid is transferred in the hydrothermal reaction kettle (14 milliliters of volumes) of polytetrafluoroethylliner liner, reactor is placed thermostat container, keep temperature to carry out hydro-thermal reaction 72h for 180 ℃.Hydro-thermal reaction gained white product moved in the dilute hydrochloric acid solution that concentration is 0.5mol/L flood 8h, carry out sufficient ion-exchange.By suction filtration, with deionized water flush away excessive hydrochloric acid, again with products therefrom 80 ℃ of oven dry, obtain intermediate product (hydrogen metatitanic acid).Gained hydrogen metatitanic acid is kept 400 ℃ of calcinings of temperature 4h in tube furnace, obtain anatase octahedrite phase and TiO
2The mixed crystal type TiO of-B phase
2Nano belt, nano belt width are 50～200nm, and length is 2～15 microns.
Conclusion: when adding 4.0g titanic oxide nano (P25), can prepare anatase octahedrite phase and TiO
2The mixed crystal type TiO of-B phase
2Nano belt, nano belt width are 50～200nm, and length is 2～15 microns.
Embodiment 8:
It is in the 10mol/L sodium hydroxide solution that 5.0g titanic oxide nano (P25) is scattered in 12 ml concns, place beaker fully to stir 30min, the gained suspension liquid is transferred in the hydrothermal reaction kettle (14 milliliters of volumes) of polytetrafluoroethylliner liner, reactor is placed thermostat container, keep temperature to carry out hydro-thermal reaction 72h for 180 ℃.Hydro-thermal reaction gained white product moved in the dilute hydrochloric acid solution that concentration is 0.5mol/L flood 8h, carry out sufficient ion-exchange.By suction filtration, with deionized water flush away excessive hydrochloric acid, again with products therefrom 80 ℃ of oven dry, obtain intermediate product (hydrogen metatitanic acid).Gained hydrogen metatitanic acid is kept 400 ℃ of calcinings of temperature 4h in tube furnace, obtain pure TiO
2The TiO of-B phase
2Nano belt, nano belt width are 50～200nm, and length is 2～15 microns.
Conclusion: when adding 5.0g titanic oxide nano (P25), can prepare pure TiO
2-B phase TiO
2Nano belt, nano belt width are 50～200nm, and length is 2～15 microns.
Embodiment 9:
It is in the 10mol/L sodium hydroxide solution that 6.0g titanic oxide nano (P25) is scattered in 12 ml concns, place beaker fully to stir 30min, the gained suspension liquid is transferred in the hydrothermal reaction kettle (14 milliliters of volumes) of polytetrafluoroethylliner liner, reactor is placed thermostat container, keep temperature to carry out hydro-thermal reaction 72h for 180 ℃.Hydro-thermal reaction gained white product moved in the dilute hydrochloric acid solution that concentration is 0.5mol/L flood 8h, carry out sufficient ion-exchange.By suction filtration, with deionized water flush away excessive hydrochloric acid, again with products therefrom 80 ℃ of oven dry, obtain intermediate product (hydrogen metatitanic acid).Gained hydrogen metatitanic acid is kept 400 ℃ of calcinings of temperature 4h in tube furnace, obtain pure TiO
2The TiO of-B phase
2Nano belt, nano belt width are 50～200nm, and length is 2～15 microns.
Conclusion: when adding 6.0g titanic oxide nano (P25), can prepare pure TiO
2-B phase TiO
2Nano belt, nano belt width are 50～200nm, and length is 2～15 microns.
Claims (4)
1. the controlled hydrothermal preparing process of a different crystal forms titanium dioxide nano-belts is 0.2～0.6: 4.8 TiO with mass ratio
2Nano powder and NaOH are raw material; With TiO
2Nano powder is scattered in the NaOH aqueous solution, stirs 20～30min, and the suspension liquid that obtains is transferred in the hydrothermal reaction kettle, carries out hydro-thermal reaction 65～75h under 170～190 ℃, obtains white product; Place HCl solution to flood 8～12h white product, carry out ion-exchange, suction filtration, with the excessive hydrochloric acid of deionized water flush away, oven dry obtains the intermediate hydrogen metatitanic acid again; The hydrogen metatitanic acid at 400 ℃ of calcinings of temperature 4h, is obtained the TiO of pure anatase octahedrite phase
2Nano belt.
2. the controlled hydrothermal preparing process of a different crystal forms titanium dioxide nano-belts is 0.8～4: 4.8 TiO with mass ratio
2Nano powder and NaOH are raw material; With TiO
2Nano powder is scattered in the NaOH aqueous solution, stirs 20～30min, and the suspension liquid that obtains is transferred in the hydrothermal reaction kettle, carries out hydro-thermal reaction 65～75h under 170～190 ℃, obtains white product; Place HCl solution to flood 8～12h white product, carry out ion-exchange, suction filtration, with the excessive hydrochloric acid of deionized water flush away, oven dry obtains the intermediate hydrogen metatitanic acid again; The hydrogen metatitanic acid is kept 400 ℃ of calcinings of temperature 4h in tube furnace, obtain anatase octahedrite phase and TiO
2The mixed crystal type TiO of-B phase
2Nano belt.
3. the controlled hydrothermal preparing process of a different crystal forms titanium dioxide nano-belts is 5～6: 4.8 TiO with mass ratio
2Nano powder and NaOH are raw material; With TiO
2Nano powder is scattered in the NaOH aqueous solution, stirs 20～30min, and the suspension liquid that obtains is transferred in the hydrothermal reaction kettle, carries out hydro-thermal reaction 65～75h under 170～190 ℃, obtains white product; Place HCl solution to flood 8～12h white product, carry out ion-exchange, suction filtration, with the excessive hydrochloric acid of deionized water flush away, oven dry obtains the intermediate hydrogen metatitanic acid again; The hydrogen metatitanic acid is kept 400 ℃ of calcinings of temperature 4h in tube furnace, obtain TiO
2The TiO of-B phase
2Nano belt.
4. according to the controlled hydrothermal preparing process of claim 1,2 or 3 described different crystal forms titanium dioxide nano-belts, it is characterized in that, described sodium hydroxide solution, concentration is 9～11mol/L; Described hydrochloric acid soln, concentration are 0.1～1mol/L.
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