CN103848457A - Nitrogen-doped anatase crystal form titanium dioxide nanopowder and preparation method thereof - Google Patents

Nitrogen-doped anatase crystal form titanium dioxide nanopowder and preparation method thereof Download PDF

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Publication number
CN103848457A
CN103848457A CN201210497038.5A CN201210497038A CN103848457A CN 103848457 A CN103848457 A CN 103848457A CN 201210497038 A CN201210497038 A CN 201210497038A CN 103848457 A CN103848457 A CN 103848457A
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nitrogen
powder
anatase crystal
doped
nano tio
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王拴
许思超
张云霞
李广海
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Hefei Institutes of Physical Science of CAS
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Hefei Institutes of Physical Science of CAS
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Abstract

The invention discloses nitrogen-doped anatase crystal form titanium dioxide nanopowder and a preparation method thereof. The powder is the nitrogen-doped anatase crystal form titanium dioxide nanopowder, wherein the atom percentage of nitrogen to anatase crystal form titanium dioxide is 1.4-2.0at%: 98.0-98.6at%, the appearance of the powder is in a shuttle shape or a rod shape, the shuttle length of the shuttle-shaped powder is 200-300nm, the shuttle diameter is 40-50 nm, the cone angle at two ends of the shuttle is 10-15 DEG, the rod length of the rod-shaped powder is 150-300nm, and the rod diameter is 50-60nm. The method comprises the following steps: dissolving the titanium nitride powder in water, stirring to obtain a titanium nitride aqueous solution, adding ammoniacal liquor and hydrogen peroxide in the titanium nitride aqueous solution according to volume ratio of 28.1-32.14: 1-8: 1.5-2.5 in order and stirring to obtain a precursor solution, reacting the precursor solution under an enclosed state to obtain a reaction solution, washing a sediment in the cooled reaction solution by using ethanol, and drying to prepare an object product. The nitrogen-doped anatase crystal form titanium dioxide nanopowder is capable of performing visible-light photocatalysis on water polluted by methylene blue.

Description

Nitrogen-doped anatase crystal formation nano TiO 2 powder and preparation method thereof
Technical field
The present invention relates to a kind of nano TiO 2 powder and preparation method, especially a kind of nitrogen-doped anatase crystal formation nano TiO 2 powder and preparation method thereof.
Background technology
Titanium dioxide is a kind of widely used wide bandgap semiconductor materials, and its stable chemical nature, nontoxic, is desirable photocatalyst material, can be widely used in the fields such as purifying air, antibacterial, sewage disposal.With respect to body phase material, based on small-size effect, surface effects, quantum size effect etc., nano titanium oxide has more excellent photocatalysis performance and chemical property.Because the energy gap of anatase crystal titanium dioxide is 3.2eV, only under the effect of UV-light, just can demonstrate obvious photocatalytic activity, and that UV-light in solar spectrum only accounts for is about 3～5%, seriously restrict its application as photocatalyst material and solar cell.For this reason, people are in order to widen the scope of anatase crystal titanium dioxide spectrum response, make unremitting effort, as " a kind of nonmetal doping nano-TiO disclosing in disclosed Chinese invention patent application Publication Specification CN 101074113 A on November 21st, 2007 2preparation method and application thereof ".The preparation method who mentions in this specification sheets, taking the nonmetallic compound of Ti as precursor, mixes and carries out hydrothermal synthesis reaction with acid, water, after it through washing, the nano-TiO that dry, grinding obtains nonmetal doping 2catalyzer, wherein, the nonmetallic compound of Ti is TiN, TiC or TiS 2; The product that preparation method makes is the nano-titanium dioxide powder existing with Anatase.But this preparation method exists weak point, first, though made nonmetal doping nano titanium oxide, fail to point out clearly the crystal formation of its pattern and titanium dioxide, the intrinsic propesties that is difficult to understand fully and bring into play product; Secondly, product only can be used for the visible light photocatalytic degradation to benzene; Finally, the existence of grinding steps has increased complicacy, time and the cost of preparation.
Summary of the invention
The technical problem to be solved in the present invention, for overcoming weak point of the prior art, provides a kind of nitrogen-doped anatase crystal formation nano TiO 2 powder that can carry out to the water that polluted by methylene blue visible light photocatalytic degradation.
Another technical problem that the present invention will solve is for providing a kind of preparation method of above-mentioned nitrogen-doped anatase crystal formation nano TiO 2 powder.
For solving technical problem of the present invention, the technical scheme adopting is: nitrogen-doped anatase crystal formation nano TiO 2 powder comprises anatase crystal nano TiO 2 powder, particularly,
In described anatase crystal nano TiO 2 powder, doped with nitrogen, described is 1.4～2.0at%:98.0～98.6at% doped with the atomic percent between nitrogen and anatase crystal titanium dioxide in the anatase crystal nano TiO 2 powder of nitrogen;
The described anatase crystal nano TiO 2 powder doped with nitrogen is shuttle shape, or bar-shaped, wherein, the shuttle length of shuttle shape powder is that 200～300nm, shuttle diameter are that the cone angle at 40～50nm, shuttle two ends is 10～15 degree, and the rod length of rod-shaped powder is that 150～300nm, excellent diameter are 50～60nm.
As the further improvement of nitrogen-doped anatase crystal formation nano TiO 2 powder, the described direction of growth doped with the anatase crystal titanium dioxide in the anatase crystal nano TiO 2 powder of nitrogen is [001] crystal orientation.
For solving another technical problem of the present invention, another technical scheme adopting is: the preparation method of above-mentioned nitrogen-doped anatase crystal formation nano TiO 2 powder adopts hydrothermal method, and particularly completing steps is as follows:
Step 1, the ratio that is first 0.1～0.14:28～32 according to weight ratio, by at least 0.5h of rear stirring soluble in water nitride powder, obtain the titanium nitride aqueous solution, be the hydrogen peroxide that 25～28% ammoniacal liquor and concentration are 25～35% to adding concentration in the titanium nitride aqueous solution successively again, and stir at least 1h, wherein, the volume ratio of the titanium nitride aqueous solution, ammoniacal liquor and hydrogen peroxide is 28.1～32.14:1～8:1.5～2.5, obtains precursor solution;
Step 2, first precursor solution is placed in to air-tight state, be at 160～180 DEG C, to react at least 12h in temperature, obtain reaction solution, again the throw out in cooled reaction solution is used after washing with alcohol, be placed on dry at least 24h at 70～90 DEG C, make nitrogen-doped anatase crystal formation nano TiO 2 powder.
As the preparation method's of nitrogen-doped anatase crystal formation nano TiO 2 powder further improvement, described water is deionized water, or distilled water; Described is 0.5～1h by the time of nitride powder rear stirring soluble in water; Described is 1～3h to adding the time of stirring after ammoniacal liquor and hydrogen peroxide in the titanium nitride aqueous solution successively; Described reaction times precursor solution being placed at 160～180 DEG C is 12～24h; The described number of times to the throw out use washing with alcohol in cooled reaction solution is 1～3 time; The dry time is 24～28h afterwards in the described washing to throw out.
Beneficial effect with respect to prior art is, one, use respectively scanning electron microscope, transmission electron microscope, X-ray diffractometer and x-ray photoelectron spectroscopy to characterize to the target product making, from its result, the target product making is numerous, monodispersed shuttle shape thing or club, wherein, the shuttle length of shuttle shape thing is that 200～300nm, shuttle diameter are that the cone angle at 40～50nm, shuttle two ends is 10～15 degree, and the rod length of club is that 150～300nm, excellent diameter are 50～60nm; Shuttle shape thing and club form by nitrogen and anatase crystal titanium dioxide, and atomic percent is between the two 1.4～2.0at%:98.0～98.6at%; The direction of growth of the anatase crystal titanium dioxide in shuttle shape thing and club is [001] crystal orientation.Its two, to be subject to methylene blue pollute water use target product carry out visible light photocatalytic degradation, use simultaneously ultraviolet-visual spectrometer to degraded characterize, from its result, the methylene blue in water has fully been decomposed.Its three, preparation method's science, effectively: both made containing other dephasigns, be only the nitrogen-doped anatase crystal formation nano TiO 2 powder of single crystal form; Again by regulating the add-on of ammoniacal liquor in precursor solution to make the control that in target product, the doping of nitrogen and the pattern of target product all can be artificial; Also make target product there is the performance of the methylene blue in water being carried out to visible light photocatalytic degradation; More do not need the technique of grinding and reduced complicacy, time and the cost prepared.
As the further embodiment of beneficial effect, the one, water is preferably deionized water, or distilled water, has avoided the introducing of impurity.The 2nd, the time of nitride powder rear stirring soluble in water is preferably to 0.5～1h, in the titanium nitride aqueous solution, add the time of stirring after ammoniacal liquor and hydrogen peroxide to be preferably 1～3h successively, the reaction times that precursor solution is placed at 160～180 DEG C is preferably 12～24h, use the number of times of washing with alcohol to be preferably 1～3 time to the throw out in cooled reaction solution, after throw out is washed, the dry time is preferably 24～28h, be and only needing, under the situation of less time or number of times, just to have guaranteed the quality of the target product making.
Brief description of the drawings
Below in conjunction with accompanying drawing, optimal way of the present invention is described in further detail.
Fig. 1 is that target product to making uses one of result that scanning electron microscope (SEM) characterizes.Wherein, the SEM image when pattern that Fig. 1 a is target product is shuttle shape, the SEM image when pattern that Fig. 1 b is target product is bar-shaped; As seen from Figure 1, target product is numerous shuttle shape thing or club.
Fig. 2 is that target product to making uses one of result that transmission electron microscope (TEM) characterizes.Wherein, Fig. 2 a is the TEM image of shuttle shape target product, and Fig. 2 b is the local high magnification TEM image of Fig. 2 a;
Can be found out by TEM image, the direction of growth of the nitrogen-doped anatase crystal formation titanium dioxide in shuttle shape target product is [001] crystal orientation.It is [001] crystal orientation too that bar-shaped target product is used to the result that transmission electron microscope characterizes.
Fig. 3 is that target product to making uses one of result that X-ray diffraction (XRD) instrument characterizes.Curve 1 in XRD spectra is the standard spectral line of anatase crystal titanium dioxide, and curve 2 is the spectral line of shuttle shape target product, the spectral line that curve 3 is bar-shaped target product; This XRD spectra has shown that the titanium dioxide in target product is anatase crystal.
Fig. 4 is that target product to making uses one of result that x-ray photoelectron power spectrum (XPS) instrument characterizes.Wherein, the XPS spectrum figure that Fig. 4 a is target product; Fig. 4 b is the 1s power spectrum spectral line of N element in XPS spectrum figure shown in Fig. 4 a having amplified, and it has confirmed in titanium dioxide doped with nitrogen element.
Fig. 5 is one of result of sign while using uv-vis spectra (UV-Vis) instrument to carry out visible light photocatalytic degradation to the hydromining target product that polluted by methylene blue.Wherein, the concentration of aqueous solution of methylene blue is 50mg/L, and the consumption of target product is 0.8mg/L, and visible light source is selected xenon lamp; Virgin curve in UV-Vis spectrogram is the spectral line without xenon lamp catalyzed degradation, and other curve is the spectral line of the xenon lamp catalyzed degradation of going through 10～60min.From UV-Vis spectrogram, xenon lamp irradiates after 60min, and the methylene blue of throwing in the water that has target product has fully been decomposed.
Embodiment
First buy from market or make by ordinary method:
Nitride powder; As deionized water and the distilled water of water; Ammoniacal liquor; Hydrogen peroxide; Ethanol.
Then,
Embodiment 1
The concrete steps of preparation are:
Step 1, the ratio that is first 0.1:32 according to weight ratio, by rear stirring 0.5h soluble in water nitride powder; Wherein, water is deionized water, obtains the titanium nitride aqueous solution.Be the hydrogen peroxide that 25% ammoniacal liquor and concentration are 35% to adding concentration in the titanium nitride aqueous solution successively again, and stir 1h; Wherein, the volume ratio of the titanium nitride aqueous solution, ammoniacal liquor and hydrogen peroxide is 28.1:8:1.5, obtains precursor solution.
Step 2, is first placed in air-tight state by precursor solution, is to react 24h at 160 DEG C in temperature, obtains reaction solution.Again to after the throw out use washing with alcohol in cooled reaction solution 1 time, be placed on dry 28h at 70 DEG C, make and be similar to Fig. 1 a, Fig. 2 a and as shown in Figure 2 b, and nitrogen-doped anatase crystal formation nano TiO 2 powder as shown in the curve in Fig. 3 and Fig. 4.
Embodiment 2
The concrete steps of preparation are:
Step 1, the ratio that is first 0.11:31 according to weight ratio, by rear stirring 0.6h soluble in water nitride powder; Wherein, water is distilled water, obtains the titanium nitride aqueous solution.Be the hydrogen peroxide that 26% ammoniacal liquor and concentration are 33% to adding concentration in the titanium nitride aqueous solution successively again, and stir 1.5h; Wherein, the volume ratio of the titanium nitride aqueous solution, ammoniacal liquor and hydrogen peroxide is 29:7:1.8, obtains precursor solution.
Step 2, is first placed in air-tight state by precursor solution, is to react 21h at 165 DEG C in temperature, obtains reaction solution.Again throw out in cooled reaction solution is used after washing with alcohol 2 times, be placed on dry 27h at 75 DEG C, make as shown in Fig. 1 a, Fig. 2 a and Fig. 2 b, and nitrogen-doped anatase crystal formation nano TiO 2 powder as shown in the curve in Fig. 3 and Fig. 4.
Embodiment 3
The concrete steps of preparation are:
Step 1, the ratio that is first 0.12:30 according to weight ratio, by rear stirring 0.75h soluble in water nitride powder; Wherein, water is deionized water, obtains the titanium nitride aqueous solution.Be the hydrogen peroxide that 26.5% ammoniacal liquor and concentration are 30% to adding concentration in the titanium nitride aqueous solution successively again, and stir 2h; Wherein, the volume ratio of the titanium nitride aqueous solution, ammoniacal liquor and hydrogen peroxide is 30:5:2, obtains precursor solution.
Step 2, is first placed in air-tight state by precursor solution, is to react 18h at 170 DEG C in temperature, obtains reaction solution.Again to after the throw out use washing with alcohol in cooled reaction solution 2 times, be placed on dry 26h at 80 DEG C, make and be similar to Fig. 1 a, Fig. 2 a and as shown in Figure 2 b, and nitrogen-doped anatase crystal formation nano TiO 2 powder as shown in the curve in Fig. 3 and Fig. 4.
Embodiment 4
The concrete steps of preparation are:
Step 1, the ratio that is first 0.13:29 according to weight ratio, by rear stirring 0.8h soluble in water nitride powder; Wherein, water is distilled water, obtains the titanium nitride aqueous solution.Be the hydrogen peroxide that 27% ammoniacal liquor and concentration are 28% to adding concentration in the titanium nitride aqueous solution successively again, and stir 2.5h; Wherein, the volume ratio of the titanium nitride aqueous solution, ammoniacal liquor and hydrogen peroxide is 31:3:2.3, obtains precursor solution.
Step 2, is first placed in air-tight state by precursor solution, is to react 15h at 175 DEG C in temperature, obtains reaction solution.Again throw out in cooled reaction solution is used after washing with alcohol 3 times, be placed on dry 25h at 85 DEG C, make as shown in Fig. 1 b and Fig. 2 b, and nitrogen-doped anatase crystal formation nano TiO 2 powder as shown in the curve in Fig. 3 and Fig. 4.
Embodiment 5
The concrete steps of preparation are:
Step 1, the ratio that is first 0.14:28 according to weight ratio, by rear stirring 1h soluble in water nitride powder; Wherein, water is deionized water, obtains the titanium nitride aqueous solution.Be the hydrogen peroxide that 28% ammoniacal liquor and concentration are 25% to adding concentration in the titanium nitride aqueous solution successively again, and stir 3h; Wherein, the volume ratio of the titanium nitride aqueous solution, ammoniacal liquor and hydrogen peroxide is 32.14:1:2.5, obtains precursor solution.
Step 2, is first placed in air-tight state by precursor solution, is to react 12h at 180 DEG C in temperature, obtains reaction solution.Again throw out in cooled reaction solution is used after washing with alcohol 3 times, be placed on dry 24h at 90 DEG C, make and be similar to Fig. 1 b and as shown in Figure 2 b, and nitrogen-doped anatase crystal formation nano TiO 2 powder as shown in the curve in Fig. 3 and Fig. 4.
The purposes of nitrogen-doped anatase crystal formation nano TiO 2 powder is,
Nitrogen-doped anatase crystal formation nano TiO 2 powder is placed in to the water that polluted by methylene blue and carries out visible light photocatalytic degradation processing, obtain the result as shown in the curve in Fig. 5.
Obviously, those skilled in the art can carry out various changes and modification and not depart from the spirit and scope of the present invention nitrogen-doped anatase crystal formation nano TiO 2 powder of the present invention and preparation method thereof.Like this, if to these amendments of the present invention with within modification belongs to the scope of the claims in the present invention and equivalent technologies thereof, the present invention is also intended to comprise these changes and modification interior.

Claims (9)

1. a nitrogen-doped anatase crystal formation nano TiO 2 powder, comprises anatase crystal nano TiO 2 powder, it is characterized in that:
In described anatase crystal nano TiO 2 powder, doped with nitrogen, described is 1.4～2.0at%:98.0～98.6at% doped with the atomic percent between nitrogen and anatase crystal titanium dioxide in the anatase crystal nano TiO 2 powder of nitrogen;
The described anatase crystal nano TiO 2 powder doped with nitrogen is shuttle shape, or bar-shaped, wherein, the shuttle length of shuttle shape powder is that 200～300nm, shuttle diameter are that the cone angle at 40～50nm, shuttle two ends is 10～15 degree, and the rod length of rod-shaped powder is that 150～300nm, excellent diameter are 50～60nm.
2. nitrogen-doped anatase crystal formation nano TiO 2 powder according to claim 1, is characterized in that doped with the direction of growth of the anatase crystal titanium dioxide in the anatase crystal nano TiO 2 powder of nitrogen be [001] crystal orientation.
3. a preparation method for nitrogen-doped anatase crystal formation nano TiO 2 powder described in claim 1, adopts hydrothermal method, it is characterized in that completing steps is as follows:
Step 1, the ratio that is first 0.1～0.14:28～32 according to weight ratio, by at least 0.5h of rear stirring soluble in water nitride powder, obtain the titanium nitride aqueous solution, be the hydrogen peroxide that 25～28% ammoniacal liquor and concentration are 25～35% to adding concentration in the titanium nitride aqueous solution successively again, and stir at least 1h, wherein, the volume ratio of the titanium nitride aqueous solution, ammoniacal liquor and hydrogen peroxide is 28.1～32.14:1～8:1.5～2.5, obtains precursor solution;
Step 2, first precursor solution is placed in to air-tight state, be at 160～180 DEG C, to react at least 12h in temperature, obtain reaction solution, again the throw out in cooled reaction solution is used after washing with alcohol, be placed on dry at least 24h at 70～90 DEG C, make nitrogen-doped anatase crystal formation nano TiO 2 powder.
4. the preparation method of nitrogen-doped anatase crystal formation nano TiO 2 powder according to claim 3, is characterized in that water is deionized water, or distilled water.
5. the preparation method of nitrogen-doped anatase crystal formation nano TiO 2 powder according to claim 3, is characterized in that by the time of nitride powder rear stirring soluble in water be 0.5～1h.
6. the preparation method of nitrogen-doped anatase crystal formation nano TiO 2 powder according to claim 3, is characterized in that successively in the titanium nitride aqueous solution, adding the time of stirring after ammoniacal liquor and hydrogen peroxide is 1～3h.
7. the preparation method of nitrogen-doped anatase crystal formation nano TiO 2 powder according to claim 3, is characterized in that the reaction times that precursor solution is placed at 160～180 DEG C is 12～24h.
8. the preparation method of nitrogen-doped anatase crystal formation nano TiO 2 powder according to claim 3, is characterized in that it is 1～3 time that the throw out in cooled reaction solution is used to the number of times of washing with alcohol.
9. the preparation method of nitrogen-doped anatase crystal formation nano TiO 2 powder according to claim 3, after it is characterized in that throw out to wash, the dry time is 24～28h.
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Cited By (3)

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CN106268896A (en) * 2015-05-12 2017-01-04 中国科学院金属研究所 A kind of nano silicon nitride titanio composite photocatalyst material and its preparation method and application
CN106698367A (en) * 2015-11-13 2017-05-24 中国科学院金属研究所 Method for preparing titanium nitride-based composite material
CN106957065A (en) * 2017-04-19 2017-07-18 中国工程物理研究院化工材料研究所 A kind of supper-fast preparation method of N, Ti3+ codope porous TiO2 nanometer sheet

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106268896A (en) * 2015-05-12 2017-01-04 中国科学院金属研究所 A kind of nano silicon nitride titanio composite photocatalyst material and its preparation method and application
CN106698367A (en) * 2015-11-13 2017-05-24 中国科学院金属研究所 Method for preparing titanium nitride-based composite material
CN106698367B (en) * 2015-11-13 2019-04-30 中国科学院金属研究所 A method of preparing nitridation titanium composite material
CN106957065A (en) * 2017-04-19 2017-07-18 中国工程物理研究院化工材料研究所 A kind of supper-fast preparation method of N, Ti3+ codope porous TiO2 nanometer sheet
CN106957065B (en) * 2017-04-19 2018-07-31 中国工程物理研究院化工材料研究所 A kind of supper-fast preparation method of N, Ti3+ codope porous TiO2 nanometer sheet

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Application publication date: 20140611