CN102701275A - Method for preparing TiO2 nano laces - Google Patents
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- CN102701275A CN102701275A CN2012101804491A CN201210180449A CN102701275A CN 102701275 A CN102701275 A CN 102701275A CN 2012101804491 A CN2012101804491 A CN 2012101804491A CN 201210180449 A CN201210180449 A CN 201210180449A CN 102701275 A CN102701275 A CN 102701275A
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Abstract
The invention discloses a method for preparing TiO2 nano laces, and belongs to the technical field of nano materials. According to the method, commercial P25 TiO2 nano particles are adopted, and are synthetized into TiO2 nano belts as precursors in a hydro-thermal method, butyl titanate solution is assed in HCl aqueous solution and uniformly mixed, a certain quantity of TiO2 nano belts is added in a mixed solution and uniformly mixed, then the mixed solution is transferred in a reaction kettle for reacting for 6 to 12 hours at the temperature of 160 to 200 DEG C, washed and dried to obtain the TiO2 nano laces; the P25 TiO2 nano particles, the TiO2 nano belts and the TiO2 nano laces are subject to the silver mixing processing in a silver mirror reaction method to obtain Ag/P25 TiO2 nano particles, Ag/TiO2 nano belts and Ag/TiO2 nano laces, and experiment that methyl orange is subject to photocatalytic degradation shows that Ag/TiO2 nano lace have strongest photocatalytic activity.
Description
Technical field
The invention belongs to technical field of nano material, particularly a kind of preparation TiO
2The method of nanometer lace.
Background technology
TiO
2Nano material has bigger specific surface area, excellent charge transport properties, is widely used in fields such as photochemical catalysis, dye sensitization solar battery and lithium celies.TiO
2Nanostructure, comprise nano particle, nano wire, nano-pillar, nano belt and nano flower-like structure etc., embody different performances, attracted numerous research.TiO
2The compound method of nanostructure adopts hydrothermal synthesis method usually, and this method preparation technology is simple, easy control of reaction conditions.Different nanostructures is controlled by different synthesis conditions, like hydrolysis rate, the concentration of titanium compound, the pH value of solution etc.Wherein, how to change synthesis condition, obtain to contain the structure at a large amount of sharp keen edges and turning, to improving TiO
2Photochemistry and catalytic performance are of crucial importance.We are through adding the TiO that has had nanostructure in reactant
2Nano belt utilizes the butyl(tetra)titanate hydrolyzed product at TiO as the carrier of reaction
2The ordering growth on nano belt surface has obtained a kind of new nanostructure.Existing compound method can realize single flower structure; The synthetic nano belt can realize the synthetic zonal bouquet that is similar to as support and this method is utilized; The spike flower of a branch of bundle is arranged on the nano belt; Thereby more help obtaining big specific surface area, have a large amount of sharpened edges and turning simultaneously, can obtain excellent photochemistry and photocatalysis performance undoubtedly.
Summary of the invention
The objective of the invention is to propose a kind of new preparation TiO
2The method of nanometer lace, method provided by the invention adopts TiO
2Nano belt is as the carrier (presoma) of reaction, and adopts simple silver mirror reaction to prepare to mix the TiO of silver
2Nanometer lace structure.Concrete preparation method comprises the steps:
(1) preparation TiO
2Nano belt:
A. with P25 TiO
2Nano particle joins in the NaOH aqueous solution, and magnetic agitation is even, and the gained mixing solutions is put into reaction kettle, and 180 ~ 200 ℃ were reacted 12 ~ 24 hours down, with the washing of gained precipitate with deionized water, suction filtration, to filtrating to neutrality, obtained the sodium titanate nano belt;
B. prepare HCl solution, the sodium titanate nano belt that step a is made is soaked in the described HCl solution;
C. with step b gained solid matter with deionized water washing, suction filtration, to filtrating for neutral, again after dry, calcining, acquisition TiO
2Nano belt;
(2) according to deionized water: volume(tric)fraction is that the volume ratio of 37% hydrochloric acid is that the ratio preparation HCl of 1:1 suppresses solution; Suppress to add in the solution ratio that massfraction is butyl(tetra)titanate solution 1 ~ 3mL of 98% according to the described HCl of every 17mL again, butyl(tetra)titanate solution is joined described HCl suppress in the solution, be stirred to evenly;
(3) in step (2) gained solution, add the TiO that an amount of step (1) makes
2Nano belt continues to be stirred to evenly;
(4) step (3) gained solution is transferred in the reaction kettle, 160 ~ 200 ℃ were reacted 6 ~ 12 hours down;
(5) be neutral with reacted precipitate with deionized water and absolute ethanol washing to filtrating, carry out drying treatment then, promptly obtain TiO
2The nanometer lace;
(6) prepare silver ammino solution under the room temperature: in reaction vessel, splash into silver nitrate solution, the concentration of silver nitrate solution is controlled between 1wt% ~ 2wt%; In reaction vessel, drip the ammoniacal liquor of concentration more gradually, the PH in the reaction vessel is controlled between 8 ~ 9 at 1wt% ~ 2wt%, and constantly concussion, disappear just until the deposition that is produced;
(7) with the TiO that makes
2The nanometer lace adds in the silver ammino solution of step (6) preparation, dropwise adds the glucose solution of 0.1 ~ 0.3mol/L then, reaction 8 ~ 10min; The compounding substances that obtains with deionized water wash, suction filtration, is neutrality until filtrating, and then after vacuumizing drying, promptly obtains Ag/TiO
2The nanometer lace.
The TiO that said step (1) makes
2Nano belt, length can reach tens microns, and width is 50 ~ 200 nanometers, and thickness is about 50 nanometers;
The concentration of the NaOH solution that uses in the said step (1) is 10mol/L, and the concentration of HCl solution is 0.1 mol/L, to guarantee carrying out fully of reaction;
Drying temperature in the said step (1) is 50 ~ 70 ℃, and be 1 ~ 3 hour time of drying; Calcining temperature is 550 ~ 650 ℃, and calcination time is 1 ~ 3 hour;
The TiO that adds in the said step (3)
2The weight of nano belt is: 17mL HCl suppresses solution in every use step (2), adds the TiO that 0.01 ~ 0.05g step (1) makes
2Nano belt;
Drying treatment in the said step (5) is: drying temperature is 80 ℃, and be 12 hours time of drying.
Beneficial effect of the present invention is:
The present invention adopts industrial TiO
2Particle (P25) at first utilizes hydrothermal method synthesis of titanium dioxide nano belt, hydro-thermal synthetic advantage be can in the control of warm liquid phase, energy consumption is relatively low, controllability good and in airtight container, carry out, and pollutes little; Utilize the TiO of method preparation provided by the present invention
2The nanometer lace has a lot of sharpened edges and turning, can effectively improve TiO
2Photochemistry and photocatalysis performance; To TiO
2The test shows of nanometer lace, TiO
2Nanometer lace structure has very big specific surface area; Photodegradation experiment according to carrying out shows TiO
2The nanometer lace is better than TiO to the photochemical catalysis effect of tropeolin-D
2With P25 and TiO
2Nano belt; Because TiO
2The nanometer lace has big specific surface area and stronger photocatalytic activity, so can be widely used in fields such as photochemistry, lithium cell test, dye sensitization and solar cell.
Description of drawings
Fig. 1 is synthetic new Ti O in the embodiment of the invention
2The scanning electron microscope diagram of nanometer lace structure;
Fig. 2 is synthetic Ag/P25, Ag/TiO in the embodiment of the invention
2Nano belt and Ag/TiO
2The comparative test result of the photocatalytic degradation methyl orange solution of nanometer lace.
Embodiment
A kind of method for preparing the nano titania lace that the present invention proposes can be implemented through following method, and concrete preparation method comprises the steps:
(1) preparation TiO
2Nano belt:
A. with P25 TiO
2Nano particle joins in the NaOH aqueous solution that concentration is 10mol/L, and magnetic agitation is even, and the gained mixing solutions is put into reaction kettle, and 180 ~ 200 ℃ were reacted 12 ~ 24 hours down, with the washing of gained precipitate with deionized water, suction filtration, is neutrality to filtrating;
B. compound concentration is the HCl solution of 0.1mol/L, and step a gained throw out is soaked in the described HCl solution;
C. with the washing of step b gained solid matter with deionized water, suction filtration, be neutral to filtrating; It is under 50 ~ 70 ℃ the condition dry 1 ~ 3 hour in temperature then; After under temperature is 550 ~ 650 ℃ condition, calcining 1 ~ 3 hour at last, promptly obtain TiO
2Nano belt;
(2) according to deionized water: volume(tric)fraction is that the volume ratio of 37% hydrochloric acid is that the ratio preparation HCl of 1:1 suppresses solution; Suppress to add in the solution ratio that massfraction is butyl(tetra)titanate solution 1 ~ 3mL of 98% according to the described HCl of every 17mL again, butyl(tetra)titanate solution is joined described HCl suppress in the solution, be stirred to evenly;
(3) suppress solution according to 17mL HCl in every use step (2), add the TiO that 0.01 ~ 0.05g step (1) makes
2The ratio of nano belt, the TiO that step (1) is made
2Nano belt joins the HCl inhibition solution that step (2) makes, and continues to be stirred to evenly;
(4) step (3) gained solution is transferred in the reaction kettle, 160 ~ 200 ℃ were reacted 6 ~ 12 hours down;
(5) with reacted precipitate with deionized water and alcohol washing to filtrating for neutral, then 80 ℃ dry 12 hours down, promptly obtain TiO
2The nanometer lace;
(6) prepare silver ammino solution under the room temperature: in reaction vessel, splash into silver nitrate solution, the concentration of silver nitrate solution is controlled between 1wt% ~ 2wt%; In reaction vessel, drip the ammoniacal liquor of concentration more gradually, the PH in the reaction vessel is controlled between 8 ~ 9 at 1wt% ~ 2wt%, and constantly concussion, disappear just until the deposition that is produced;
(7) with the TiO that makes
2The nanometer lace adds in the silver ammino solution of step (6) preparation, dropwise adds the glucose solution of 0.1 ~ 0.3mol/L then, reaction 8 ~ 10min; The compounding substances that obtains with deionized water wash, suction filtration, is neutrality until filtrating, and then after vacuumizing drying, promptly obtains Ag/TiO
2The nanometer lace.
Below in conjunction with concrete embodiment the present invention is done detailed explanation:
Embodiment 1:
(1) preparation TiO
2Nano belt:
A. with 1g P25 TiO
2Nano particle joins in the NaOH aqueous solution that 100mL concentration is 10mol/L, and magnetic agitation is even, and the gained mixing solutions is put into reaction kettle, and 200 ℃ were reacted 24 hours down, with the washing of gained precipitate with deionized water, suction filtration, is neutrality to filtrating;
B. compound concentration is the HCl solution 250mL of 0.1mol/L, and step a gained throw out is soaked in the described HCl solution;
C. with the washing of step b gained solid matter with deionized water, suction filtration, be neutral to filtrating; Under 60 ℃ condition dry 2 hours then, promptly obtain TiO in calcining under 600 ℃ the condition after 2 hours at last
2Nano belt;
(2) according to deionized water: volume(tric)fraction is that the volume ratio of 37% hydrochloric acid is that the ratio preparation HCl of 1:1 suppresses solution 17mL, and suppressing to add in the solution massfraction to described HCl then is 98% butyl(tetra)titanate solution 1.5mL, is stirred to evenly;
(3) in above-mentioned solution, add the TiO that 0.02g step (1) prepares
2Nano belt continues to stir about 10min to even;
(4) step (3) gained solution is transferred in the reaction kettle, 160 ℃ were reacted 6 hours down;
(5) with reacted precipitate with deionized water and alcohol washing to filtrating for neutral, then 80 ℃ dry 12 hours down, promptly obtain the TiO shown in accompanying drawing 1
2The nanometer lace;
(6) three parts of the silver ammino solutions of preparation 0.2mol/L, the P25 TiO of weighing 0.1g respectively under the room temperature
2Nano particle, the TiO of step (1) preparation
2Nano belt and TiO
2The nanometer lace places silver ammino solution respectively;
(7) glucose solution with 0.3mol/L dropwise splashes in the solution of step (6) preparation silver mirror reaction 10min; Three parts of compounding substances that obtain are used deionized water wash, suction filtration respectively, for neutral, after under 80 ℃ of conditions dry 6 hours, obtain Ag/P25, Ag/ TiO then until filtrating
2Nano belt and Ag/ TiO
2The nanometer lace;
(8) with the Ag/P25 that makes in the step (7), Ag/ TiO
2Nano belt and Ag/ TiO
2The nanometer lace carries out the experiment of photocatalytic degradation tropeolin-D respectively, and concrete grammar is following: configuration concentration is the methyl orange solution of 0.02g/L under the room temperature; Get three parts of the methyl orange solutions of 20mL preparation, the Ag/P25 that respectively 0.02g is made, Ag/ TiO
2Nano belt and Ag/TiO
2The nanometer lace joins in the described methyl orange solution, and uv illumination 60min carries out the photoabsorption test to the sample that obtains then.The result is as shown in Figure 2, and the result shows: Ag/ TiO
2The nanometer lace demonstrates the strongest photocatalytic activity, simultaneously Ag/ TiO
2The photocatalysis performance of nano belt also is superior to Ag/ P25.
The TiO that the step (1) that adds in embodiment 1 step (3) is made
2Nano belt changes 0.01g, 0.03g, 0.04g or 0.05g into, and other conditions are with embodiment 1, can both obtain the technique effect same like embodiment 1.
Claims (6)
1. one kind prepares TiO
2The method of nanometer lace is characterized in that, concrete preparation method comprises the steps:
(1) preparation TiO
2Nano belt:
A. with P25 TiO
2Nano particle joins in the NaOH aqueous solution, and magnetic agitation is even, and the gained mixing solutions is put into reaction kettle, and 180 ~ 200 ℃ were reacted 12 ~ 24 hours down, with the washing of gained precipitate with deionized water, suction filtration, to filtrating to neutrality, obtained the sodium titanate nano belt;
B. prepare HCl solution, the sodium titanate nano belt that step a is made is soaked in the described HCl solution;
C. with step b gained solid matter with deionized water washing, suction filtration, to filtrating for neutral, again after dry, calcining, acquisition TiO
2Nano belt;
(2) according to deionized water: volume(tric)fraction is that the volume ratio of 37% hydrochloric acid is that the ratio preparation HCl of 1:1 suppresses solution; Suppress to add in the solution ratio that massfraction is butyl(tetra)titanate solution 1 ~ 3mL of 98% according to the described HCl of every 17mL again, butyl(tetra)titanate solution is joined described HCl suppress in the solution, be stirred to evenly;
(3) in step (2) gained solution, add the TiO that an amount of step (1) makes
2Nano belt continues to be stirred to evenly;
(4) step (3) gained solution is transferred in the reaction kettle, 160 ~ 200 ℃ were reacted 6 ~ 12 hours down;
(5) be neutral with reacted precipitate with deionized water and absolute ethanol washing to filtrating, carry out drying treatment then, promptly obtain TiO
2The nanometer lace.
2. preparation TiO according to claim 1
2The method of nanometer lace is characterized in that, the concentration of the NaOH solution that uses in the said step (1) is 10mol/L, and the concentration of HCl solution is 0.1 mol/L.
3. preparation TiO according to claim 1
2The method of nanometer lace is characterized in that, the drying temperature in the said step (1) is 50 ~ 70 ℃, and be 1 ~ 3 hour time of drying; Calcining temperature is 550 ~ 650 ℃, and calcination time is 1 ~ 3 hour.
4. preparation TiO according to claim 1
2The method of nanometer lace is characterized in that, the TiO that adds in the said step (3)
2The weight of nano belt is: 17mL HCl suppresses solution in every use step (2), adds the TiO that 0.01 ~ 0.05g step (1) makes
2Nano belt.
5. preparation TiO according to claim 1
2The method of nanometer lace is characterized in that, the drying treatment in the said step (5) is: drying temperature is 80 ℃, and be 12 hours time of drying.
6. preparation TiO according to claim 1
2The method of nanometer lace is characterized in that, described TiO
2The nanometer lace is through silver-plated processing, and described silver-plated processing comprises the steps:
(1) in reaction vessel, splash into silver nitrate solution, the concentration of silver nitrate solution is controlled between 1wt% ~ 2wt%;
(2) in reaction vessel, drip the ammoniacal liquor of concentration more gradually, the pH in the reaction vessel is controlled between 8 ~ 9 at 1wt% ~ 2wt%, and constantly concussion, disappear just until the deposition that is produced;
(3) with the TiO that makes
2The nanometer lace adds in the silver ammino solution of step (2) preparation, dropwise adds the glucose solution of 0.1 ~ 0.3mol/L then, reaction 8 ~ 10min; The compounding substances that obtains with deionized water wash, suction filtration, is neutrality until filtrating, and then after vacuumizing drying, promptly obtains Ag/TiO
2The nanometer lace.
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Cited By (10)
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| CN103318955A (en) * | 2013-06-24 | 2013-09-25 | 华北电力大学 | String-shaped TiO2 micro-sphere material and preparation method thereof |
| CN103752312A (en) * | 2013-12-26 | 2014-04-30 | 深圳大学 | Photocatalyst and preparation method thereof |
| CN103803644A (en) * | 2012-11-14 | 2014-05-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method for controlling product crystal form and morphology of titanium-based nanometer material |
| CN103880072A (en) * | 2014-03-24 | 2014-06-25 | 华北电力大学 | Preparation method of pinecone-shaped TiO2 nanomaterial |
| CN104190458A (en) * | 2014-07-16 | 2014-12-10 | 上海工程技术大学 | Low-temperature preparation process for dual-element modified nanometer TiO2 sol |
| CN105177671A (en) * | 2015-08-19 | 2015-12-23 | 苏州榕绿纳米科技有限公司 | Method for preparing silver nanoparticle/titanium dioxide nanotube array |
| CN103691433B (en) * | 2013-12-10 | 2016-01-20 | 北京科技大学 | A kind of Ag doped Ti O 2material, and its preparation method and application |
| CN106582591A (en) * | 2016-11-17 | 2017-04-26 | 广东工业大学 | Preparation method of quadrangular anatase type TiO2 |
| CN107308927A (en) * | 2017-06-28 | 2017-11-03 | 陕西科技大学 | A kind of preparation method of titanium dioxide homojunction nano-photocatalyst |
| CN107389736A (en) * | 2017-05-22 | 2017-11-24 | 江苏时瑞电子科技有限公司 | A kind of preparation method of the humidity sensor based on sodium titanate |
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| CN103803644B (en) * | 2012-11-14 | 2016-08-17 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of preparation method controlling titanium-based nano material product form and pattern |
| CN103318955A (en) * | 2013-06-24 | 2013-09-25 | 华北电力大学 | String-shaped TiO2 micro-sphere material and preparation method thereof |
| CN103318955B (en) * | 2013-06-24 | 2015-08-12 | 华北电力大学 | A kind of string-like TiO 2sphere material and preparation method thereof |
| CN103691433B (en) * | 2013-12-10 | 2016-01-20 | 北京科技大学 | A kind of Ag doped Ti O 2material, and its preparation method and application |
| CN103752312A (en) * | 2013-12-26 | 2014-04-30 | 深圳大学 | Photocatalyst and preparation method thereof |
| CN103880072A (en) * | 2014-03-24 | 2014-06-25 | 华北电力大学 | Preparation method of pinecone-shaped TiO2 nanomaterial |
| CN103880072B (en) * | 2014-03-24 | 2016-01-06 | 华北电力大学 | A kind of preparation method of pinecone shape titanium dioxide nano material |
| CN104190458A (en) * | 2014-07-16 | 2014-12-10 | 上海工程技术大学 | Low-temperature preparation process for dual-element modified nanometer TiO2 sol |
| CN105177671A (en) * | 2015-08-19 | 2015-12-23 | 苏州榕绿纳米科技有限公司 | Method for preparing silver nanoparticle/titanium dioxide nanotube array |
| CN105177671B (en) * | 2015-08-19 | 2018-05-08 | 苏州榕绿纳米科技有限公司 | A kind of preparation method of silver Nano granule/titanium dioxide nano-tube array |
| CN106582591A (en) * | 2016-11-17 | 2017-04-26 | 广东工业大学 | Preparation method of quadrangular anatase type TiO2 |
| CN107389736A (en) * | 2017-05-22 | 2017-11-24 | 江苏时瑞电子科技有限公司 | A kind of preparation method of the humidity sensor based on sodium titanate |
| CN107308927A (en) * | 2017-06-28 | 2017-11-03 | 陕西科技大学 | A kind of preparation method of titanium dioxide homojunction nano-photocatalyst |
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