CN104998630A - Titanium dioxide/graphene nanocomposite, and normal-temperature preparation method and application thereof - Google Patents

Titanium dioxide/graphene nanocomposite, and normal-temperature preparation method and application thereof Download PDF

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CN104998630A
CN104998630A CN201510354461.3A CN201510354461A CN104998630A CN 104998630 A CN104998630 A CN 104998630A CN 201510354461 A CN201510354461 A CN 201510354461A CN 104998630 A CN104998630 A CN 104998630A
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graphene
titanium dioxide
normal temperature
titanium
graphite oxide
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吴俊星
吴子华
谢华清
朱月琴
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Shanghai Polytechnic University
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Shanghai Polytechnic University
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Abstract

The invention discloses a titanium dioxide/graphene nanocomposite, and a normal-temperature preparation method and application thereof. According to the invention, a titanium source and graphite oxide are used as starting raw materials, an organic solvent is used as a reaction solvent, and the nanocomposite formed by compounding of titanium dioxide nanometer rods and graphene is obtained through normal temperature reduction and hydrolysis; and in the nanocomposite, graphene accounts for 1 to 30 wt%, with the rest being titanium dioxide. The preparation method provided by the invention has the advantages of simple process, easy preparation, mild reaction conditions, etc. In the prepared nanocomposite, titanium oxide is uniformly distributed on the surface of graphene, so the nanocomposite can be perfectly applied to the field of photocatalysis of photoelectric materials.

Description

A kind of titanium dioxide/graphene nano composite material, normal temperature preparation method and application thereof
Technical field
The present invention relates to nano material preparation and application technical field, specifically, relate to a kind of titanium dioxide/graphene nano composite material, normal temperature preparation method and application thereof.
Background technology
Titanium dioxide (TiO 2) be a kind of important stablizing and the catalysis material of environmentally safe, also there is very high chemical stability, heat endurance, nontoxic, super hydrophilic, non-migratory, and can with Food Contact, have important application prospect in fields such as power conversion, dielectric material, sensor, lithium battery, solar cell, coating, cosmetics, catalyst, photocatalytic degradations.
Titanic oxide material intercalation potential is high, and formed without SEI film in first charge-discharge process, energy conversion efficiency is higher; There is not lithium metal or alloy in titanic oxide material, security is high in charge and discharge process; Titanic oxide material crystal structure in cyclic process does not change, good stability.Titanic oxide material can be used as the good negative material of lithium-ion-power cell.But because titanic oxide material is a kind of semi-conducting material, thus electron conduction is poor, rate charge-discharge poor performance.
The titanium dioxide with plurality of advantages is also study the highest catalysis material of the most extensive, concerned degree in numerous catalysis material, be considered to one of the most promising catalysis material, the scientific research that new development in particularly having applied with new synthesis route, new method of modifying, sensitization solar battery since the 90's and nanosecond science and technology are representative, has established the leading position of titanium dioxide in catalysis material further massively.Although titanium dioxide based photocatalytic material meets the basic demand as a kind of excellent catalysis material, it is high and without visible light-responded two bottlenecks that extensive use is not still limited by the photocatalysis efficiency of material own.Many bibliographical informations employing new carbon such as CNT, fullerene etc. are compounded to form composite with titanium dioxide, due to both synergies, enhance the photocatalysis performance of material to organic matter, pollutant.Material with carbon element-titanium dioxide possesses several reasons of more superior photo-catalysis capability: the specific area that (1) composite is larger improves material
The adsorption capacity of material to organic pollution; (2) formation of material with carbon element-titanium dioxide interface hetero-junctions improves the compound between light induced electron and hole; (3) compared to pure titinium dioxide, the fermi level of composite to the direction skew of corrigendum, and then may improve the utilization rate to longer wavelength photon; (4) after carbon material surface absorb photons, titanium dioxide conduction band will be electronically injected to, form reaction exciton (the superoxide radical O in order to degradable organic pollutant 2-and Hydroxyl radical HO.
Graphene [bibliography 1: K.S.Novoselov, A.K.Geim, S.V.Morozov, D.Jiang, Y. Zhang, S.V.Dubonos, I.V.Grigorieva, A.A.Firsov.Electric field effect inatomically thin carbon films.Science, 2004,306 (5696): 666-669] be known the hardest the thinnest nano material, special cellular monoatomic layer, can the two dimensional surface material of at room temperature stable existence.There is unique thermodynamics, electric property.Graphene nanocomposite material is the complex of Graphene and nano particle, this composite property has possessed the two-fold advantage of Graphene and nano material, as special physics, and the character such as chemistry and machinery.Graphene composite material is the key areas in Graphene application study, and its prospect is boundless.
The current method preparing titanium dioxide/graphene composite material, mostly be first prepare titanium dioxide, add graphite oxide afterwards to react, and then obtain titanium dioxide/graphene compound, or first prepared titanium dioxide/graphene oxide compound, recycling reducing agent reduces, and obtains titanium dioxide/graphene compound.Namely the method that current great majority prepare titanium dioxide/graphene compound is substep preparation, and uses poisonous hydrazine hydrate etc. and be used as reducing agent.
Summary of the invention
Poisonous reducing agent is used in order to solve existing preparation in the preparation method of titanium dioxide/graphene compound, the technical problem that reduction process need heat, the object of the present invention is to provide a kind of titanium dioxide/graphene composite material, normal temperature preparation method and application thereof.The inventive method experimental implementation can prepare titanium dioxide/graphene compound at normal temperatures.Experimental implementation is more simple, mild condition, energy-conserving and environment-protective.Simultaneously the titanium dioxide/graphene complex stabilities that obtains of this method is good, and soilless sticking, difficulty comes off, and can have fine application in photoelectric material photocatalysis field.
The invention provides a kind of normal temperature preparation method of titanium dioxide/graphene nano composite material, it comprises graphite oxide
Under inorganic reducing agent effect, normal temperature reduction obtains Graphene and titanium salt ordinary-temp hydrolysis in graphene dispersing solution is obtained titanium dioxide/graphene composite nano materials two step; Wherein: described inorganic reducing agent is sodium borohydride or vulcanized sodium.
Normal temperature preparation method concrete steps provided by the invention are as follows:
(1) normal temperature reduction-oxidation graphite
Graphite oxide is placed in organic solvent, and ultrasonic disperse 0.2 ~ 1 hour, adds inorganic reducing agent, stirs 30 ~ 60 hours under room temperature condition; Filtered by gained solution afterwards, use organic solvent washing 3 ~ 5 times, filter cake alcohol disperses, and obtains graphene dispersing solution;
(2) titanium dioxide/graphene composite nano materials is prepared
First titanium salt is joined in the graphene dispersing solution that step (1) obtains, stir 2 ~ 3 hours, then in above-mentioned mixed liquor, add hydrolysis inhibitor, continue stirring 5 ~ 20 hours, and then add deionized water, stir 2 ~ 5 days; After reaction terminates, suction filtration, organic solvent washing, drying obtains titanium dioxide/graphene composite nano materials; Wherein:
The weight ratio 1 of described graphite oxide, inorganic reducing agent and titanium salt: (0.5 ~ 3): (50 ~ 500); The mass ratio of titanium salt and hydrolysis inhibitor is 1:0.05 ~ 1:0.3; The mass ratio of titanium salt and deionized water is 1:0.1 ~ 1:0.3.
In above-mentioned steps (1), step (2), described organic solvent is selected from any one or two kinds of in ethanol or isopropyl alcohol.
In above-mentioned steps (1), described graphite oxide adopts Hummers method to prepare; The mass ratio of described graphite oxide and organic solvent is 1:300 ~ 1:1000.
In above-mentioned steps (2), described titanium salt is selected from any one or several in butyl titanate, titanium sulfate or tetraisopropyl titanate; Described hydrolysis inhibitor is selected from one or more in glacial acetic acid, hydrochloric acid, sulfuric acid or nitric acid.
In above-mentioned steps (2), drying condition is: dry at 50 ~ 200 DEG C of temperature under vacuum.
The titanium dioxide/graphene nano composite material that the present invention also provides above-mentioned normal temperature preparation method to obtain, in this composite, titanium dioxide is dispersed in graphenic surface, and described titanium dioxide is that rule is bar-shaped, is of a size of 10 ~ 300nm; Preferably, in composite, the ratio shared by Graphene is 1 ~ 30wt%, and all the other are titanium dioxide; Preferred further, the ratio shared by Graphene is 1 ~ 10wt%.
The titanium dioxide/graphene nano composite material that the present invention also provides above-mentioned normal temperature preparation method to obtain further is in the application of power lithium-ion battery material or field of solar energy utilization.
Beneficial effect of the present invention is:
1, the present invention carrys out the acidity of regulation system by adding acid in preparation process, make after adding deionized water, suppressed on the one hand the fast hydrolyzing of titanium salt presoma by acid, titanium salt presoma is slowly hydrolyzed, obtain the less and more uniform composite of distribution of particle diameter;
2, avoid in preparation process using organic reducing agent, replace with inorganic reducing agent, react under normal temperature, avoid high temperature
React the heating problems brought, made preparation method both simple, low energy consumption again, the preparation for titanium dioxide and graphene composite material provides a feasible path;
3, titanium dioxide is dispersed in graphenic surface in the composite, good stability, soilless sticking, and difficulty comes off.Titanium dioxide/graphene composite material of the present invention can be used as good catalysis material, solar cell material, lithium ion battery material.
Accompanying drawing explanation
Fig. 1 is the combination product infrared spectrogram of example 1.
Fig. 2 is example 1 combination product scanning electron microscope (SEM) photograph.
Fig. 3 is example 1 combination product scanning electron microscope (SEM) photograph.
Fig. 4 is the combination product infrared spectrogram of example 2.
Fig. 5 is example 2 combination product scanning electron microscope (SEM) photograph.
Fig. 6 is the combination product infrared spectrogram of example 3.
Fig. 7 is example 3 combination product scanning electron microscope (SEM) photograph.
Detailed description of the invention
By reference to the accompanying drawings the present invention is described in further detail below by embodiment, but does not therefore limit the present invention within described scope of embodiments.
In the embodiment of the present invention, graphite oxide is prepared by Hummers method, specific as follows:
1 g graphite powder is joined in the ice-water bath containing 1 g sodium nitrate and the 20 mL concentrated sulfuric acids (98%), magnetic stirring 20 min, under stirring, add 3g potassium permanganate, and 1h is stirred under room temperature environment, 90mL ultra-pure water is added in above-mentioned solution, in 95 DEG C of backflow 15 min, dilute with ultra-pure water after being cooled to room temperature, and add 20 mL H2O2 (30%), now solution becomes yellowish-brown, by the solution suction filtration obtained, and with milli-Q water to neutral, product is dried in 60 DEG C of vacuum drying ovens, obtains graphite oxide.
Embodiment 1
1, raw materials weighing: graphite oxide and ethanol mass ratio are 1:300, graphite oxide and sodium borohydride, the mass ratio of butyl titanate is 1:2:300, butyl titanate and hydrolysis inhibitor (glacial acetic acid) mass ratio are 1:0.3, butyl titanate with deionized water quality than being 1:0.3;
2, the graphite oxide taken by step 1 is in ethanol, and ultrasonic disperse process 0.5 hour, obtains graphene oxide suspension, at ambient temperature magnetic agitation;
3, join in the graphene oxide suspension of step 2 by the sodium borohydride that step 1 takes, room temperature lower magnetic force stirs 20 hours, is washed by gained solution with ethanol, is dissolved by filter cake ethanol after filtration, obtains graphene dispersing solution;
4, the tetra-n-butyl titanate that step 1 takes to be joined in step 3 gained graphene dispersing solution magnetic agitation 2 hours, add hydrolysis inhibitor (glacial acetic acid) afterwards in the solution, magnetic agitation added deionized water after 10 hours, stirred and obtained composite organic solution in 3 days;
5, step 4 gained solution with ethanol is washed 4 times, 50 DEG C, the filter cake vacuum oven dry will obtained afterwards.Grinding obtains titanium dioxide/graphene composite material again.Fig. 1 is the combination product infrared spectrogram of example 1.Fig. 2, Fig. 3 are example 1 combination product scanning electron microscope (SEM) photograph.Result shows, and its titanium dioxide is that rule is bar-shaped;
6, by step 5 gained composite, the oven dry of 200 DEG C, vacuum.High temperature 600 DEG C calcining in atmosphere afterwards, mass change before and after weighing, calculating Graphene content is 8wt%.
Embodiment 2
1, raw materials weighing: graphite oxide and ethanol mass ratio are 1:500, graphite oxide and vulcanized sodium, the mass ratio of butyl titanate is 1:0.5:300, butyl titanate and hydrolysis inhibitor (36.7wt% hydrochloric acid) mass ratio are 1:0.2, butyl titanate with deionized water quality than being 1:0.1;
2, the graphite oxide taken by step 1 is in isopropyl alcohol, and ultrasonic disperse process 0.5 hour, obtains graphene oxide suspension, at ambient temperature magnetic agitation;
3, join in the graphene oxide suspension of step 2 by the sodium borohydride that step 1 takes, room temperature lower magnetic force stirs 30 hours, is washed by gained solution with ethanol, is dissolved by filter cake isopropyl alcohol after filtration, obtains graphene dispersing solution;
4, the butyl titanate that step 1 takes to be joined in step 3 gained graphene dispersing solution magnetic agitation 2 hours, add hydrolysis inhibitor (36.7wt% hydrochloric acid) afterwards in the solution, magnetic agitation added deionized water after 10 hours, stirred and obtained composite organic solution in 3 days;
5, step 4 gained solution with ethanol is washed 5 times, 80 DEG C, the filter cake vacuum oven dry will obtained afterwards.Grinding obtains titanium dioxide/graphene composite material again.Fig. 4 is the combination product infrared spectrogram of example 2, and Fig. 5 is example 2 combination product ESEM;
6, by step 5 gained composite, the oven dry of 200 DEG C, vacuum.High temperature 600 DEG C calcining in atmosphere afterwards, mass change before and after weighing, calculating Graphene content is 5.6wt%.
Embodiment 3
1, raw materials weighing: graphite oxide and ethanol mass ratio are 1:800, graphite oxide and sodium borohydride, the mass ratio of titanium sulfate is 1:0.5:300, titanium sulfate and hydrolysis inhibitor (30wt%H 2sO 4) mass ratio is 1:0.3, titanium sulfate is 1:0.2 with deionized water quality ratio;
2, the graphite oxide taken by step 1 is in ethanol, and ultrasonic disperse process 1 hour, obtains graphene oxide suspension, at ambient temperature magnetic agitation;
3, join in the graphene oxide suspension of step 2 by the sodium borohydride that step 1 takes, room temperature lower magnetic force stirs 30 hours, is washed by gained solution with ethanol, is dissolved by filter cake ethanol after filtration, obtains graphene dispersing solution;
4, the titanium sulfate that step 1 takes to be joined in step 3 gained graphene dispersing solution magnetic agitation 4 hours, add hydrolysis inhibitor (30wt%H in the solution afterwards 2sO 4), magnetic agitation added deionized water after 20 hours, stirred and obtained composite organic solution in 5 days;
5, step 4 gained solution with ethanol is washed 4 times, 150 DEG C, the filter cake vacuum oven dry will obtained afterwards.Grinding obtains titanium dioxide/graphene composite material again.Fig. 5 is the combination product infrared spectrogram of example 3.Fig. 6 is example 3 combination product scanning electron microscope (SEM) photograph;
6, by step 5 gained composite, the oven dry of 200 DEG C, vacuum.High temperature 600 DEG C calcining in atmosphere afterwards, mass change before and after weighing, calculating Graphene content is 5wt%.
Embodiment 4
1, raw materials weighing: graphite oxide and isopropyl alcohol alcohol mass ratio are 1:1000, graphite oxide and sodium borohydride, the mass ratio of butyl titanate is 1:0.5:500, butyl titanate and hydrolysis inhibitor (glacial acetic acid) mass ratio are 1:0.3, butyl titanate with deionized water quality than being 1:0.3;
2, the graphite oxide taken by step 1 is in isopropyl alcohol, and ultrasonic disperse process 1 hour, obtains graphene oxide suspension, at ambient temperature magnetic agitation;
3, join in the graphene oxide suspension of step 2 by the sodium borohydride that step 1 takes, room temperature lower magnetic force stirs 30 hours, is washed by gained solution with ethanol, is dissolved by filter cake ethanol after filtration, obtains graphene dispersing solution;
4, the tetra-n-butyl titanate that step 1 takes to be joined in step 3 gained graphene dispersing solution magnetic agitation 5 hours, add hydrolysis inhibitor (acetic acid) afterwards in the solution, magnetic agitation added deionized water after 30 hours, stirred and obtained composite organic solution in 5 days;
5, step 4 gained solution washed with isopropyl alcohol 1 time, ethanol are washed 3 times, 50 DEG C, the filter cake vacuum oven dry will obtained afterwards.Grinding obtains titanium dioxide/graphene composite material again;
6, by step 5 gained composite, the oven dry of 200 DEG C, vacuum.High temperature 600 DEG C calcining in atmosphere afterwards, mass change before and after weighing, calculating Graphene content is 5wt%.
Embodiment 5
1, raw materials weighing: graphite oxide and isopropyl alcohol mass ratio are 1:800, graphite oxide and sodium borohydride, the mass ratio of tetraisopropyl titanate is 1:3:50, tetraisopropyl titanate and hydrolysis inhibitor (acetic acid) mass ratio are 1:0.3, tetraisopropyl titanate with deionized water quality than being 1:0.3;
2, the graphite oxide taken by step 1 is in isopropyl alcohol, and ultrasonic disperse process 1 hour, obtains graphene oxide suspension, at ambient temperature magnetic agitation;
3, join in the graphene oxide suspension of step 2 by the sodium borohydride that step 1 takes, room temperature lower magnetic force stirs 30 hours, is washed by gained solution with ethanol, is dissolved by filter cake isopropyl alcohol after filtration, obtains graphene dispersing solution;
4, the tetraisopropyl titanate that step 1 takes to be joined in step 3 gained graphene dispersing solution magnetic agitation 5 hours, add hydrolysis inhibitor (acetic acid) afterwards in the solution, magnetic agitation added deionized water after 30 hours, stirred and obtained composite organic solution in 5 days;
5, by step 4 gained solution organic solvent washing 4 times, 50 DEG C, the filter cake vacuum oven dry will obtained afterwards.Grinding obtains titanium dioxide/graphene composite material again;
6, by step 5 gained composite, the oven dry of 200 DEG C, vacuum.High temperature 600 DEG C calcining in atmosphere afterwards, mass change before and after weighing, calculating Graphene content is 4.8wt%.

Claims (10)

1. a normal temperature preparation method for titanium dioxide/graphene nano composite material, is characterized in that, it comprises graphite oxide
Under inorganic reducing agent effect, normal temperature reduction obtains Graphene and titanium salt ordinary-temp hydrolysis in graphene dispersing solution is obtained titanium dioxide/graphene composite nano materials two step; Wherein: described inorganic reducing agent is sodium borohydride or vulcanized sodium.
2. normal temperature preparation method according to claim 1, is characterized in that, concrete steps are as follows:
(1) normal temperature reduction-oxidation graphite
Graphite oxide is placed in organic solvent, and ultrasonic disperse 0.2 ~ 1 hour, adds inorganic reducing agent, stirs 30 ~ 60 hours under room temperature condition; Filtered by gained solution afterwards, use organic solvent washing 3 ~ 5 times, filter cake organic solvent dispersion, obtains graphene dispersing solution;
(2) titanium dioxide/graphene composite nano materials is prepared
First titanium salt is joined in the graphene dispersing solution that step (1) obtains, stir 2 ~ 3 hours, then in above-mentioned mixed liquor, add hydrolysis inhibitor, continue stirring 5 ~ 20 hours, and then add deionized water, stir 2 ~ 5 days; After reaction terminates, suction filtration, organic solvent washing, drying obtains titanium dioxide/graphene composite nano materials; Wherein:
The weight ratio 1 of described graphite oxide, inorganic reducing agent and titanium salt: (0.5 ~ 3): (50 ~ 500); The mass ratio of titanium salt and hydrolysis inhibitor is 1:0.05 ~ 1:0.3; The mass ratio of titanium salt and deionized water is 1:0.1 ~ 1:0.3.
3. normal temperature preparation method according to claim 2, is characterized in that, in step (1), step (2), described in have
In machine solvent selected from ethanol or isopropyl alcohol any one or two kinds of.
4. normal temperature preparation method according to claim 2, is characterized in that, in step (1), described graphite oxide adopts Hummers method to prepare; The mass ratio of described graphite oxide and organic solvent is 1:300 ~ 1:1000.
5. normal temperature preparation method according to claim 2, is characterized in that, in step (2), described titanium salt is selected from metatitanic acid
In four butyl esters, titanium sulfate or tetraisopropyl titanate any one or several; Described hydrolysis inhibitor is selected from one or more in glacial acetic acid, hydrochloric acid, sulfuric acid or nitric acid.
6. normal temperature preparation method according to claim 2, is characterized in that: in step (2), drying condition is: vacuum
Dry at lower 50 ~ 200 DEG C of temperature.
7. according to the titanium dioxide/graphene nano composite material that the normal temperature preparation method one of claim 1-5 Suo Shu obtains, it is characterized in that, in this composite, titanium dioxide is dispersed in graphenic surface, described titanium dioxide is that rule is bar-shaped, is of a size of 10 ~ 300nm.
8. titanium dioxide/graphene nano composite material according to claim 6, is characterized in that, the ratio shared by Graphene is 1 ~ 30wt%, and all the other are titanium dioxide.
9. titanium dioxide/graphene nano composite material according to claim 7, is characterized in that, the ratio shared by Graphene is
1~ 10wt%。
10. the titanium dioxide/graphene nano composite material obtained according to the normal temperature preparation method one of claim 1-5 Suo Shu is in the application of power lithium-ion battery material or field of solar energy utilization.
CN201510354461.3A 2015-06-25 2015-06-25 Titanium dioxide/graphene nanocomposite, and normal-temperature preparation method and application thereof Pending CN104998630A (en)

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CN105289657A (en) * 2015-11-30 2016-02-03 湘潭大学 Preparation method for graphene and antimony sulphide nano-rod composite visible light catalyst
US20190247840A1 (en) * 2018-02-09 2019-08-15 Jason Yan Photocatalyst composition
CN110124509A (en) * 2018-02-09 2019-08-16 燕成祥 Light catalyst composition
CN111792669A (en) * 2020-06-02 2020-10-20 杭州电子科技大学 TiO 22Nano-rod/multilayer graphene composite material and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN105289657A (en) * 2015-11-30 2016-02-03 湘潭大学 Preparation method for graphene and antimony sulphide nano-rod composite visible light catalyst
US20190247840A1 (en) * 2018-02-09 2019-08-15 Jason Yan Photocatalyst composition
CN110124509A (en) * 2018-02-09 2019-08-16 燕成祥 Light catalyst composition
CN111792669A (en) * 2020-06-02 2020-10-20 杭州电子科技大学 TiO 22Nano-rod/multilayer graphene composite material and preparation method thereof
CN111792669B (en) * 2020-06-02 2022-07-12 杭州电子科技大学 TiO 22Nano-rod/multilayer graphene composite material and preparation method thereof

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