CN104495918B - The preparation method of particulate titanium dioxide/two-dimensional nano titanium carbide composite - Google Patents
The preparation method of particulate titanium dioxide/two-dimensional nano titanium carbide composite Download PDFInfo
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Abstract
The preparation method of particulate titanium dioxide/two-dimensional nano titanium carbide composite, adopts vacuum-sintering to prepare high-purity ternary layered Ti3AlC2Ceramic block, high-energy ball milling obtains the Ti of particle diameter at 8 μ m-75 μ m3AlC2Ceramic powder; By Ti3AlC2Ceramic powder is immersed in hydrofluoric acid solution and stirs, and corrosion reaction is eccentric cleaning again, obtains two-dimensional layer nano material MXene-Ti3C2; Finally generate TiO by tetrabutyl titanate hydrolysis2Load MXene-Ti3C2, obtain TiO2/MXene-Ti3C2Nano composite material, it is simple that the present invention has preparation process, and technique is controlled, and cost is low. Have the feature of class Graphene two-dimensional layer concurrently, MXene-Ti3C2Lamella even, specific area is large, electric conductivity is good, TiO2Particle is tiny and be evenly distributed, and the feature such as photocatalysis performance is good, and one's own physical property is good, is conducive to the application in fields such as photocatalysis, wastewater treatment, lithium ion battery, ultracapacitor, biology sensors.
Description
Technical field
The invention belongs to nano-functional material preparation field, be specifically related to a kind of graininess Detitanium-ore-type dioxyChange the preparation method of titanium/two-dimensional nano titanium carbide (MXene) composite.
Background technology
Ti3AlC2The compound between a kind of special metal and pottery, simultaneously with metal and potteryPremium properties. Both there is metallicity, at normal temperatures, had good heat conductivility and electric conductivity,There are lower vickers microhardness and higher elastic modelling quantity and modulus of shearing, can carry out machining,And there is plasticity under higher temperature; There is again ceramic performance, have higher yield strength, height simultaneouslyFusing point, high thermal stability and good non-oxidizability. Weed out the old and bring forth the new, by ternary layered Ti3AlC2Carry out corrosion research, thereby form typical two dimensional crystal MXene-Ti3C2Nano material.
Two-dimensional layer nano-carbide MXene-Ti3C2The material of a kind graphene-structured, ultra-thin twoDimension nanometer sheet due to its unique appearance structure, less particle size, larger surface volume than and formerThe synusia thickness of sub level and have superpower catalytic performance, photovoltaic performance and chemical property, makes pottery in functionThe aspects such as porcelain, photocatalysis, lithium ion battery, solar cell, gas sensor have obtained widely shouldWith.
Nano titanium oxide has most valuable optical property, all shows in auto industry and numerous areasGo out fine development prospect. Nano titanium oxide has very high chemical stability, heat endurance, nontoxicProperty etc., be widely used in anti-ultraviolet material, photocatalysis catalyst, lithium battery etc.
The people such as week prepare graphene-based titanium dioxide nano composite material and have studied its photocatalytic activity, realTest result and show, the photocatalytic activity of graphene-based titanium dioxide obviously strengthens; MichaelNaguib etc.People adopts the method such as hydro-thermal and Quick Oxidation to prepare TiO2/ graphite nano composite material, and showIts performance at the aspect such as lithium ion battery, photocatalysis is all better than single two-dimensional nano MXene-Ti3C2。
Therefore, anatase titanium dioxide/two-dimensional layer nano titanium carbide (MXene) composite, willBeing expected to has in fields such as photocatalysis, wastewater treatment, lithium ion battery, ultracapacitor, biology sensorsWell application.
Summary of the invention
In order to overcome the defect of above-mentioned prior art, the object of the invention is to pass through tetrabutyl titanate hydrolysisGenerate TiO2Load to MXene-Ti3C2Nano-material surface, thus a kind of graininess Detitanium-ore-type two is providedThe preparation method of titanium oxide/two-dimensional nano titanium carbide (MXene) composite, by Ti3AlC2In HF acidIn carry out chemical etching, Al is selectively etched away, form a kind of two-dimensional layer material MXene-Ti3C2，Then at two-dimensional layer material MXene-Ti3C2Upper load TiO2, make MXene-Ti3C2Obtain specific surface larger,Take into account TiO2Advantage, as photocatalysis performance, one's own physical property, pattern is various etc.
In order to achieve the above object, technical scheme of the present invention is as follows:
The preparation method of graininess anatase titanium dioxide/two-dimensional nano titanium carbide composite, comprise asLower step:
(1) by ternary layered Ti3AlC2Ceramic powder high-energy ball milling 1h-4h, rotating speed 400r/min, ballMaterial mass ratio 10:1,40 DEG C of-60 DEG C of oven dry after refinement powder, obtain the Ti of particle diameter at 8 μ m-75 μ m3AlC2Ceramic powder;
(2) by gained Ti in step (1)3AlC2Ceramic powder is got 2g～10g and is immersed in 50mL～200mLIn 35wt%～45wt% hydrofluoric acid solution, react 6h～120h; Stir, by corrosion product with deionized water fromThe heart cleans, until centrifuged supernatant pH is between 5～6; Then clean 2～4 times with absolute ethyl alcohol; WillGained solid sample is dry, obtains two-dimensional layer nano material MXene-Ti3C2；
(3) by step (2) gained two-dimensional nano MXene-Ti3C2Get 150mg～250mg and put into 200mLIn absolute ethyl alcohol, stir 0.5h, splash into the butyl titanate of 0.5mL～2mL, continue to stir 6h, useAbsolute ethyl alcohol eccentric cleaning is extremely decomposed without titanium dioxide, then uses deionized water eccentric cleaning, by solid sampleDry, obtain TiO2/MXene-Ti3C2Composite.
Advantage of the present invention is to utilize simple chemical reaction tetrabutyl titanate hydrolysis, at room temperature comparativelyProduce efficiently TiO2Load Balanced, the TiO that pattern is various2/MXene-Ti3C2Composite. TiO2Load, has improved single MXene-Ti3C2The various performances of powder, it will be more extensive making its application. ForFurther in the application in the fields such as ultracapacitor, lithium ion battery, biology sensor, nano adsorber,Carry out the preparation work of predecessor.
Brief description of the drawings
Fig. 1 is Ti3AlC2Before powder corrosion treatment, after corrosion treatment, and corrosion product MXene-Ti3C2Load TiO2The XRD collection of illustrative plates of sample.
Fig. 2 (a) is Ti3AlC2The SEM figure of powder granule, Fig. 2 (b) is MXene-Ti after corrosion treatment3C2SEM figure, Fig. 2 (c) is TiO2/MXene-Ti3C2The SEM figure of nano composite material, Fig. 2 (d)For the local high power SEM figure of Fig. 2 (c).
Detailed description of the invention
Further describe the present invention by specific embodiments below, the present invention also can not taking off by otherScheme from the technology of the present invention feature is described, therefore within the scope of the present invention all or be equal to model of the present inventionChange in enclosing is all included in the invention.
Embodiment mono-
The present embodiment comprises the following steps:
(1) adopt the method for vacuum-sintering to prepare highly purified ternary layered Ti3AlC2Ceramic powder, thenHigh-energy ball milling powder 4h, rotating speed 400r/min, ball material mass ratio 10:1,60 DEG C of oven dry after refinement powder,See Fig. 1 and Fig. 2 (a), in Fig. 1, XRD collection of illustrative plates has illustrated that the thing of gained powder is Ti mutually3AlC2Crystal,And impurity content is few, in Fig. 2 (a), SEM figure has shown Ti3AlC2The microscopic appearance of crystal, canFind out that its grain size is about 8 μ m, and obvious layer structure;
(2) gained powder 5g in step (1) is immersed in 100mL, 40wt% hydrofluoric acid solution and is reacted48h, stir, by corrosion product deionized water eccentric cleaning, until centrifuged supernatant pH 5～6 itBetween; Then clean 4 times with absolute ethyl alcohol; By gained solid sample drying at room temperature, obtain two-dimensional layer and receiveRice material MXene-Ti3C2, see Fig. 1, wherein XRD collection of illustrative plates has shown Ti3AlC2The variation of diffraction maximum,XRD diffracting spectrum contrast with theory is calculated, successfully obtains MXene-Ti3C2Powder thing phase. SeeFig. 2 (b), wherein SEM figure has shown MXene-Ti3C2Microscopic appearance, can find out its sheet bed thicknessDegree is about 50nm, is typical two-dimensional layer nano material;
(3) by step (2) gained two-dimensional nano MXene-Ti3C2Get 200mg and put into the anhydrous second of 200mLIn alcohol, stir 0.5h, splash into the butyl titanate of 1mL, continue to stir 6h, centrifugal with absolute ethyl alcoholClean to decomposing without titanium dioxide, then use deionized water eccentric cleaning, solid sample is dried, to obtain final productTiO2/MXene-Ti3C2Composite. See Fig. 1, wherein XRD collection of illustrative plates has shown Detitanium-ore-type TiO2Crystal successfully loads to MXene-Ti3C2On powder. See Fig. 2 (c) and Fig. 2 (d), wherein SEMFigure has shown TiO2/MXene-Ti3C2The microscopic appearance of composite, can find out TiO2Size is about25nm, and be evenly distributed, load to well MXene-Ti3C2In two-dimensional layer nano material, formNovel TiO2/MXene-Ti3C2Nano composite material.
Embodiment bis-
The present embodiment comprises the following steps:
(1) adopt the method for vacuum-sintering to prepare highly purified ternary layered Ti3AlC2Ceramic powder, thenHigh-energy ball milling powder 1h, rotating speed 400r/min, ball material mass ratio 10:1,40 DEG C of oven dry after refinement powder,Obtain Ti3AlC2Ceramic powder;
(2) gained powder 2g in step (1) is immersed in 50mL, 35wt% hydrofluoric acid solution and is reacted6h, stirs, and washed with de-ionized water is about 5～6 to pH, and absolute ethyl alcohol cleans 2 times, centrifugation,Gained solid sample is dry, obtain two-dimensional layer MXene-Ti3C2Nano material;
(3) by step (2) gained two-dimensional nano MXene-Ti3C2Get 150mg and put into 200mL absolute ethyl alcohol,Stir 0.5h, splash into the butyl titanate of 0.5mL, continue to stir 6h, use absolute ethyl alcohol eccentric cleaning to nothingTitanium dioxide decomposes, then uses deionized water eccentric cleaning, and solid sample is dried, and obtains TiO2/MXene-Ti3C2Composite.
Embodiment tri-
The present embodiment comprises the following steps:
(1) adopt the method for vacuum-sintering to prepare highly purified ternary layered Ti3AlC2Ceramic powder, thenHigh-energy ball milling powder 3h, rotating speed 400r/min, ball material mass ratio 10:1,50 DEG C of oven dry after refinement powder;
(2) gained powder 3g in step (1) is immersed in 70mL, 35wt% hydrofluoric acid solution and is reacted24h, stir, by corrosion product deionized water eccentric cleaning, until centrifuged supernatant pH 5～6 itBetween; Then clean 3 times with absolute ethyl alcohol; Gained solid sample is dry, obtain two-dimensional layer nanometer materialMaterial MXene-Ti3C2；
(3) by step (2) gained two-dimensional nano MXene-Ti3C2Get 150mg and put into the anhydrous second of 200mLIn alcohol, stir 0.5h, splash into the butyl titanate of 1.5mL, continue to stir 6h, centrifugal with absolute ethyl alcoholClean to decomposing without titanium dioxide, then use deionized water eccentric cleaning, solid sample is dried, to obtain final productTiO2/MXene-Ti3C2Composite.
Embodiment tetra-
The present embodiment comprises the following steps:
(1) adopt the method for vacuum-sintering to prepare highly purified ternary layered Ti3AlC2Ceramic powder, thenHigh-energy ball milling powder 3h, rotating speed 400r/min, ball material mass ratio 10:1,50 DEG C of oven dry after refinement powder;
(2) gained powder 4g in step (1) is immersed in 90mL, 40wt% hydrofluoric acid solution and is reacted48h, stir, by corrosion product deionized water eccentric cleaning, until centrifuged supernatant pH 5～6 itBetween; Then clean 4 times with absolute ethyl alcohol; Gained solid sample is dry, obtain two-dimensional layer nanometer materialMaterial MXene-Ti3C2；
(3) by step (2) gained two-dimensional nano MXene-Ti3C2Get 200mg and put into 200mL absolute ethyl alcohol,Stir 0.5h, splash into the butyl titanate of 2mL, continue to stir 6h, use absolute ethyl alcohol eccentric cleaning to nothingTitanium dioxide decomposes, then uses deionized water eccentric cleaning, and solid sample is dried, and to obtain final productTiO2/MXene-Ti3C2Composite.
Claims (1)
1. the preparation method of graininess anatase titanium dioxide/two-dimensional nano titanium carbide composite, itsBe characterised in that, comprise the steps:
(1) by ternary layered Ti3AlC2Ceramic powder high-energy ball milling 1h-4h, rotating speed 400r/min, ballMaterial mass ratio 10:1,40 DEG C of-60 DEG C of oven dry after refinement powder, obtain the Ti of particle diameter at 8 μ m-75 μ m3AlC2Ceramic powder;
(2) by gained Ti in step (1)3AlC2Ceramic powder is got 2g～10g submergence 50mL～200mLIn 35wt%～45wt% hydrofluoric acid solution, react 6h～120h; Stir, by corrosion product with deionized water fromThe heart cleans, until centrifuged supernatant pH is between 5～6; Then clean 2～4 times with absolute ethyl alcohol; WillGained solid sample is dry, obtains two-dimensional layer nano material MXene-Ti3C2；
(3) by step (2) gained two-dimensional nano MXene-Ti3C2Get 150mg～250mg and put into 200mLIn absolute ethyl alcohol, stir 0.5h, splash into the butyl titanate of 0.5mL～2mL, continue to stir 6h, useAbsolute ethyl alcohol eccentric cleaning is extremely decomposed without titanium dioxide, then uses deionized water eccentric cleaning, by solid sampleDry, obtain TiO2/MXene-Ti3C2Composite.
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