CN107934965A - A kind of Ti3C2‑Co(OH)(CO3)0.5The preparation method of nanocomposite - Google Patents

A kind of Ti3C2‑Co(OH)(CO3)0.5The preparation method of nanocomposite Download PDF

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CN107934965A
CN107934965A CN201711350994.XA CN201711350994A CN107934965A CN 107934965 A CN107934965 A CN 107934965A CN 201711350994 A CN201711350994 A CN 201711350994A CN 107934965 A CN107934965 A CN 107934965A
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CN107934965B (en
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武文玲
卫丹
朱建锋
崔云
方园
王芬
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Shaanxi University of Science and Technology
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Abstract

A kind of Ti3C2‑Co(OH)(CO3)0.5The preparation method of nanocomposite, first, concentration be 40wt% HF solution in selective corrosion fall ternary Ti3AlC2The Al layers of ceramic powder, form two-dimensional layer Ti3C2Nano material；Then, with two-dimentional Ti3C2Nano material is matrix, with Co (NO3)2·6H2O is cobalt source, CO (NH2)2After precipitating reagent uniform stirring, the various Ti of pattern is successfully prepared in 80 85 DEG C of growth in situ by hydro-thermal method in mixed liquor3C2@Co(OH)(CO3)0.5Nanocomposite；And assemble them into the ultracapacitor of three-electrode system, Ti3C2‑Co(OH)(CO3)0.5It is demonstrated by good chemical property；This methods experiment process is simple, cost is low, environmentally friendly, Co (OH) (CO3)0.5Pattern is beneficial to control, is Ti3C2‑Co(OH)(CO3)0.5Application in terms of ultracapacitor, lithium ion battery is laid a good foundation.

Description

A kind of Ti3C2-Co(OH)(CO3)0.5The preparation method of nanocomposite
Technical field
It is more particularly to a kind of the invention belongs to nano-functional material and the preparing technical field of electrochemical energy storage materials Ti3C2-Co(OH)(CO3)0.5The preparation method of nanocomposite.
Background technology
New Two Dimensional material MXene is the transition metal carbonitrides or carbide of a species graphene-structured, such as Ti3C2、 Ti2C etc..Ti3C2Nano material removes MAX phases Ti by HF selective corrosions3AlC2In Al layer elements be made, and can keep former It is constant to carry out MAX structures.Two-dimentional carbide Ti3C2Good stability, larger specific surface area, high bending strength and springform Amount, excellent electric property and electric conductivity, imply that this material can as the desired matrix of composite material, electrochemistry, The fields such as composite material enhancing have a extensive future.
The method that Naguib et al. uses acid etch, by Ti3AlC2When complete wetting is certain in hydrofluoric acid at room temperature Between after, Al atomic layers are fully exfoliated out.
Maria et al. presses Ti3C2：Conductive agent：Binding agent mass ratio=85%:10%:5% ratio is adopted in KOH solution With three electrode asymmetric systems to Ti3C2Chemical property characterized.Test result indicates that Ti3C2Volume and capacity ratio exist Up to 340F/cm in KOH solution3, and interlamellar spacing increases.
Sun et al. is by Ti3C2As li-ion electrode negative material, test result shows, under the multiplying power of 1 C, lithium ion For battery capacity up to 123.6mAh/g, coulombic efficiency is about 47%.But Ti3C2Theoretical specific capacity is smaller, causes its electrochemistry Can be not good enough, application of the MXene bases in the energy storage such as ultracapacitor and lithium ion battery field also needs further to be studied.
Basic cobaltous carbonate Co (OH) (CO3)0.5It is to prepare nano Co3O4The good presoma of material, therefore obtain in recent years The extensive concern of people.Basic cobaltous carbonate is heated easy decomposition, but its catabolite impurity is few, so being highly suitable for various cobalts The processing and manufacturing of material, is commonly used for the additive of electronic material, magnetic material.In recent years in subcarbonate crystal structure, heat The research of stability and surface nature etc. has made significant progress.But the research in terms of its chemical property So far it is also immature.
Zhou W.J. et al. are by electrochemical deposition method by active material Co (OH)2Be deposited directly on matrix, and by its Working electrode as ultracapacitor is tested, and specific capacitance is up to 1084F/g.
Document is searched for, it is found that not yet someone utilizes Co (OH) (CO so far3)0.5To improve Ti3C2Chemical property.This hair It is bright with good conductivity, constitutionally stable two dimension Ti3C2Ceramic powder is matrix, with Co (NO3)2·6H2O is cobalt source, CO (NH2)2 For precipitating reagent, PVP successfully prepares Ti by hydro-thermal method as structure directing agent in 80-85 DEG C of growth in situ3C2@Co(OH) (CO3)0.5Nanocomposite.And assemble them into the ultracapacitor of three-electrode system, Ti3C2-Co(OH)(CO3)0.5Performance Good chemical property, and experimentation of the present invention is simple, product morphology is controllable, safety and environmental protection, is it further in lithium The application in the energy storage such as ion battery and ultracapacitor field is laid a good foundation.
The content of the invention
The defects of in order to overcome the above-mentioned prior art, it is an object of the invention to provide a kind of Ti3C2-Co(OH) (CO3)0.5The preparation method of nanocomposite, utilizes hydro-thermal method growth in situ Co (OH) (CO3)0.5It is various that pattern is prepared Ti3C2-Co(OH)(CO3)0.5Nanocomposite, this methods experiment process is simple, cost is low, environmentally friendly, Co (OH) (CO3)0.5Pattern is beneficial to control, and increases Ti3C2Specific surface area, improve electrode material for super capacitor.
To achieve these goals, the technical solution adopted by the present invention is：
A kind of Ti3C2-Co(OH)(CO3)0.5The preparation method of nanocomposite, comprises the following steps：
Step 1, prepares ternary Ti3AlC2Ceramic powder；
Step 2, prepares two-dimensional layer Ti3C2Nano material；
Step 3, a kind of Ti3C2-Co(OH)(CO3)0.5The preparation of nanocomposite；
First, by 145.5-1164mg Co (NO3)2·6H2The O and two-dimensional layer Ti obtained by step (2)3C2Nano-powder 200mg is dissolved in ultra-pure water, successively adds 100-800mg CO (NH under magnetic stirring2)2Persistently stirred with 200-1600g PVP Mix 0.5-2h and obtain mixed liquor；Secondly, volume fraction is transferred to the hydrothermal reaction kettle polytetrafluoroethyl-ne of 100ml for 75% mixed liquor In alkene liner, the hydrothermal reaction kettle assembled is warming up to 80-85 DEG C of insulation 6-12h；Then, by the production of cooled to room temperature Thing centrifuges cleaning 3 times respectively with ultra-pure water and absolute ethyl alcohol successively, and each 4000-6000r/min centrifuges 3-5min；Most Afterwards, in vacuum drying chamber required Ti is obtained after 40 DEG C of dry 12-24h3C2@Co(OH)(CO3)0.5Nanocomposite.
Step 4, Ti3C2-Co(OH)(CO3)0.5The preparation of electrode；
First, nickel foam is cut into 1*2cm2The rectangle of size, weighs the active material of 160-200mg i.e. successively Ti obtained by step 33C2@Co(OH)(CO3)0.5Nano-powder, the conductive acetylene of 20-30mg is black, the poly- difluoro second partially of 1-10mg Alkene, grinds 1-2h in agate mortar；Secondly, after drawing the NMP grindings uniformly of 300 μ L with liquid-transfering gun, slurry mean droplet is added in In the nickel foam cut, and by the nickel foam being added dropwise in vacuum drying chamber 60-80 DEG C of dry 12-24h；Again, will make Good electrode slice 15-20Mpa pressurizes 1min under tablet press machine both obtains Ti3C2@Co(OH)(CO3)0.5Electrode.
The step one prepares ternary layered Ti3AlC2Ceramic powder, is specially：First, it is Ti according to molar ratio：Al： TiC=1.0：1.2：2.0 ratio mixes three kinds of raw materials；Secondly, three kinds of raw materials are placed in ball grinder, are made with alumina balls For abrasive media, absolute ethyl alcohol is 900 revs/min as ball-milling additive, drum's speed of rotation, is ball according to mass ratio：Material：Ethanol =3.0：1.0：1.0 ratio, general milling 1h obtains uniform powder, and is baked in 40 DEG C of freeze-day with constant temperature baking ovens；Then, Dried batch mixing is placed in corundum crucible, using the method for vacuum non-pressure sintering, is heated to the heating rate of 8 DEG C/min 1350 DEG C, 1h is kept the temperature, room temperature is cooled to the furnace and obtains high-purity Ti3AlC2Ceramic powder.
Finally, to Ti3AlC2Ceramic powder carries out wet method high-energy ball milling 3h, and every 30 minutes once, rotating speed 400r/min, steel The mass ratio of ball and ceramic powder is 10:1, levigate powder is sieved, that is, obtains the ternary Ti that particle diameter is less than 38 μm3AlC2Pottery Porcelain powder.
The step two prepares two-dimensional layer Ti3C2Nano material, is specially：Take gained in 5g step (1) Ti3AlC2Ceramic powder is slowly immersed in 100mL 40wt% hydrofluoric acid solutions, to not after effervescent by its magnetic force at room temperature 48h, rotating speed 1200r/min are stirred, when by corrosion product with deionized water eccentric cleaning to supernatant pH value being about 5-6, then Centrifuged 4 times with absolute ethyl alcohol, black precipitate is finally dried in vacuo 24h in 40 DEG C, that is, obtains two-dimensional layer Ti3C2Nano-powder.
Product is verified：
Using three-electrode system, with Ti3C2@Co(OH)(CO3)0.5As working electrode, platinized platinum is used as to electrode, silver electrode Silver chlorate is reference electrode, and under the KOH electrolyte of 6M, Ti is tested using Shanghai Chen Hua CHI660E electrochemical workstations3C2@Co (OH)(CO3)0.5The chemical property of electrode, such as cyclic voltammetry curve, constant current charge-discharge, AC impedance. Ti3C2-Co(OH) (CO3)0.5Good chemical property is demonstrated by, CV curve maps are preferable close to regular rectangle, symmetry；Cyclic curve institute shape Into region increase with the increase of sweep speed, but the general shape of figure is basically unchanged, and shows good multiplying power Performance.
Beneficial effects of the present invention：
1st, ternary Ti is fallen in selective corrosion to the present invention first in the HF solution that concentration is 40wt%3AlC2Ceramic powder Al layers, form two-dimensional layer Ti3C2Nano material.Then, with two-dimentional Ti3C2Nano material is matrix, with Co (NO3)2·6H2O For cobalt source, CO (NH2)2After precipitating reagent uniform stirring, mixed liquor is successfully prepared by hydro-thermal method in 80-85 DEG C of growth in situ Ti3C2@Co(OH)(CO3)0.5Nanocomposite.And the ultracapacitor of three-electrode system is assembled them into, it is molten with 6M KOH Liquid is as electrolyte, Ti3C2-Co(OH)(CO3)0.5It is used as working electrode, platinum electrode and electrode, silver/silver chloride electrode is made Cyclic voltammetry, Ti are carried out for reference electrode3C2-Co(OH)(CO3)0.5It is demonstrated by good chemical property, and the present invention Experimentation is simple, and product morphology is controllable, safety and environmental protection, is that it further leads in the energy storage such as lithium ion battery and ultracapacitor The application in domain is laid a good foundation.
2nd, by the various Ti of the pattern being prepared3C2-Co(OH)(CO3)0.5Nanocomposite is as ultracapacitor Active electrode, tested on CHI660E electrochemical workstations, illustrate its good chemical property, be Ti3C2- Co(OH)(CO3)0.5Application in terms of ultracapacitor, lithium ion battery is laid a good foundation.
Brief description of the drawings
Fig. 1 is Ti3C2-Co(OH)(CO3)0.5The XRD diagram of nanocomposite, wherein tetra- curves of a, b, c, d are respectively The XRD diagram of embodiment one, two, three, four.
Fig. 2 is Ti3C2-Co(OH)(CO3)0.5The SEM figures of nanocomposite, wherein a, b, c, d are respectively embodiment First, two, three, four SEM figures.
Fig. 3 is three Ti of embodiment3C2-Co(OH)(CO3)0.5Nanocomposite different scanning rates under three-electrode system Cyclic voltammetry curve figure.
Embodiment
The present invention is described in further details with embodiment below in conjunction with the accompanying drawings.
Embodiment one
The present embodiment comprises the following steps：
Step 1, ternary Ti3AlC2The preparation of ceramic powder；
Method according to patent ZL201310497696.9 prepares ternary layered Ti3AlC2Ceramic powder：First, according to rubbing Your ratio is Ti：Al：TiC=1.0：1.2：2.0 ratio mixes three kinds of raw materials；Secondly, three kinds of raw materials are placed in ball grinder, Using alumina balls as abrasive media, absolute ethyl alcohol is as ball-milling additive, and drum's speed of rotation is 900 revs/min, according to mass ratio For ball：Material：Ethanol=3.0：1.0：1.0 ratio, general milling 1h obtain uniform powder, and will in 40 DEG C of freeze-day with constant temperature baking ovens It is dried；Then, dried batch mixing is placed in corundum crucible, using the method for vacuum non-pressure sintering, with the liter of 8 DEG C/min Warm speed is heated to 1350 DEG C, keeps the temperature 1h, cools to room temperature with the furnace and obtain high-purity Ti3AlC2Ceramic powder.
Finally, to Ti3AlC2Ceramic powder carries out wet method high-energy ball milling 3h, and every 30 minutes once, rotating speed 400r/min, steel The mass ratio of ball and ceramic powder is 10:1, levigate powder is sieved, that is, obtains the Ti that particle diameter is less than 38 μm3AlC2Ceramic powder Body.
Step 2, two-dimensional layer Ti3C2The preparation of nano material；
Method according to patent 201410812056.7 prepares two-dimensional layer Ti3C2Nano material:Take in 5g step (1) Gained Ti3AlC2Ceramic powder is slowly immersed in 100mL 40wt% hydrofluoric acid solutions, to not after effervescent by it at room temperature Magnetic agitation 48h, rotating speed 1200r/min, with deionized water eccentric cleaning to supernatant pH value are about 5-6 by corrosion product When, then centrifuged 4 times with absolute ethyl alcohol.Black precipitate is finally dried in vacuo 24h in 40 DEG C, that is, obtains two-dimensional layer Ti3C2Nanometer Powder.
Step 3, a kind of Ti3C2-Co(OH)(CO3)0.5The preparation of nanocomposite；
First, by 1164mg Co (NO3)2·6H2The O and Ti obtained by step (2)3C2Nano-powder 200mg is dissolved in ultra-pure water In, 800mg CO (NH are successively added under magnetic stirring2)22h, which is persistently stirred, with 1600mg PVP obtains mixed liquor；Secondly, will Volume fraction is transferred in the hydrothermal reaction kettle polytetrafluoroethyllining lining of 100ml for 75% mixed liquor, and the hydro-thermal assembled is anti- Kettle is answered to be warming up to 82 DEG C of insulation 8h；Then, by the product of cooled to room temperature successively with ultra-pure water and absolute ethyl alcohol respectively from Heart separation cleaning 3 times, each 4000-6000r/min centrifuge 3-5min；Finally, in vacuum drying chamber after 40 DEG C of dry 24h Obtain required Ti3C2@Co(OH)(CO3)0.5Nanocomposite.It can be seen that from a curves of Fig. 1 in 2 θ=36 °, 42 °, 62 ° correspond respectively to (111), (200), outside the characteristic peak of the Ti3C2 of (220) crystal face, also in 2 θ=18 °, and 25 °, 34 ° of correspondences In Co (OH) (CO that PDF standard cards number are 48-00833)0.5(020), (111), the diffraction maximum of (221) crystal face.Show Ti is successfully prepared by hydro-thermal method3C2@presomas Co (OH) (CO3)0.5Composite material.From a figures of Fig. 2 it can be seen that coming, by Load capacity is too many in reaction system, Co (OH) (CO3)0.5In Ti3C2The thicker wrapping layer of Surface Creation, Co (OH) (CO3)0.5In nano-sheet, and self assembly is in anthogram picture.
Step 4, Ti3C2-Co(OH)(CO3)0.5The preparation of electrode；
First, nickel foam is cut into 1*2cm2The rectangle of size, weighs the active material i.e. step of 200mg successively Three gained Ti3C2@Co(OH)(CO3)0.5Nano-powder, the conductive acetylene of 20mg is black, and the polyvinylidene fluoride of 1mg, grinds in agate 1-2h is ground in alms bowl；Secondly, after drawing the NMP grindings uniformly of 300 μ L with liquid-transfering gun, slurry mean droplet is added in the foam cut On nickel, and by the nickel foam being added dropwise in vacuum drying chamber 60 DEG C of dry 24h；Again, by the electrode slice made in tablet press machine Lower 15Mpa pressurizes 1min both obtains Ti3C2@Co(OH)(CO3)0.5Electrode.
Three-electrode system is finally used, with Ti3C2@Co(OH)(CO3)0.5Electrode is used as to electricity as working electrode, platinized platinum Pole, silver-colored silver chlorate is reference electrode, under the KOH electrolyte of 6M, is tested using Shanghai Chen Hua CHI660E electrochemical workstations Ti3C2@Co(OH)(CO3)0.5The chemical property of electrode, such as cyclic voltammetry curve, constant current charge-discharge, AC impedance.
Embodiment two
The present embodiment comprises the following steps：
Step 1, ternary Ti3AlC2The preparation of ceramic powder；
Method according to patent ZL201310497696.9 prepares ternary layered Ti3AlC2Ceramic powder：First, according to rubbing Your ratio is Ti：Al：TiC=1.0：1.2：2.0 ratio mixes three kinds of raw materials；Secondly, three kinds of raw materials are placed in ball grinder, Using alumina balls as abrasive media, absolute ethyl alcohol is as ball-milling additive, and drum's speed of rotation is 900 revs/min, according to mass ratio For ball：Material：Ethanol=3.0：1.0：1.0 ratio, general milling 1h obtain uniform powder, and will in 40 DEG C of freeze-day with constant temperature baking ovens It is dried；Then, dried batch mixing is placed in corundum crucible, using the method for vacuum non-pressure sintering, with the liter of 8 DEG C/min Warm speed is heated to 1350 DEG C, keeps the temperature 1h, cools to room temperature with the furnace and obtain high-purity Ti3AlC2Ceramic powder.
Finally, to Ti3AlC2Ceramic powder carries out wet method high-energy ball milling 3h, and every 30 minutes once, rotating speed 400r/min, steel The mass ratio of ball and ceramic powder is 10:1, levigate powder is sieved, that is, obtains the Ti that particle diameter is less than 38 μm3AlC2Ceramic powder Body.
Step 2, two-dimensional layer Ti3C2The preparation of nano material；
Method according to patent 201410812056.7 prepares two-dimensional layer Ti3C2Nano material:Take in 5g step (1) Gained Ti3AlC2Ceramic powder is slowly immersed in 100mL 40wt% hydrofluoric acid solutions, to not after effervescent by it at room temperature Magnetic agitation 48h, rotating speed 1200r/min, with deionized water eccentric cleaning to supernatant pH value are about 5-6 by corrosion product When, then centrifuged 4 times with absolute ethyl alcohol.Black precipitate is finally dried in vacuo 24h in 40 DEG C, that is, obtains two-dimensional layer Ti3C2Nanometer Powder.
Step 3, a kind of Ti3C2-Co(OH)(CO3)0.5The preparation of nanocomposite；
First, by 727.6mg Co (NO3)2·6H2The O and Ti obtained by step (2)3C2Nano-powder 200mg is dissolved in ultrapure In water, 500mg CO (NH are successively added under magnetic stirring2)22h, which is persistently stirred, with 1000mg PVP obtains mixed liquor；Secondly, Volume fraction is transferred in the hydrothermal reaction kettle polytetrafluoroethyllining lining of 100ml for 75% mixed liquor, the hydro-thermal that will be assembled Reaction kettle is warming up to 82 DEG C of insulation 8h；Then, the product of cooled to room temperature is distinguished with ultra-pure water and absolute ethyl alcohol successively Cleaning 3 times is centrifuged, each 4000-6000r/min centrifuges 3-5min；Finally, 40 DEG C of dry 24h in vacuum drying chamber After obtain required Ti3C2@Co(OH)(CO3)0.5Nanocomposite.It can be seen that from the b curves of Fig. 1 in 2 θ=36 °, 42 °, 62 ° correspond respectively to (111), (200), outside the characteristic peak of the Ti3C2 of (220) crystal face, also in 2 θ=18 °, and 25 °, 34 ° of correspondences In Co (OH) (CO that PDF standard cards number are 48-00833)0.5(020), (111), the diffraction maximum of (221) crystal face.Show Ti is successfully prepared by hydro-thermal method3C2@presomas Co (OH) (CO3)0.5Composite material.From the b figures of Fig. 2 it can be seen that coming, by Load capacity is still too many in reaction system, Co (OH) (CO3)0.5In Ti3C2The thicker wrapping layer of Surface Creation, Co (OH) (CO3)0.5In nanometer wire.
Step 4, Ti3C2-Co(OH)(CO3)0.5The preparation of electrode；
First, nickel foam is cut into 1*2cm2The rectangle of size, weighs the active material i.e. step of 200mg successively Three gained Ti3C2@Co(OH)(CO3)0.5Nano-powder, the conductive acetylene of 2mg is black, the polyvinylidene fluoride of 1mg, in agate mortar Middle grinding 1-2h；Secondly, after drawing the NMP grindings uniformly of 300 μ L with liquid-transfering gun, slurry mean droplet is added in the nickel foam cut On, and by the nickel foam being added dropwise in vacuum drying chamber 60 DEG C of dry 24h；Again, by the electrode slice made under tablet press machine 15Mpa pressurizes 1min both obtains Ti3C2@Co(OH)(CO3)0.5Electrode.
Three-electrode system is finally used, with Ti3C2@Co(OH)(CO3)0.5Electrode is used as to electricity as working electrode, platinized platinum Pole, silver/silver chlorate is reference electrode, under the KOH electrolyte of 6M, is tested using Shanghai Chen Hua CHI660E electrochemical workstations Ti3C2@Co(OH)(CO3)0.5The chemical property of electrode, such as cyclic voltammetry curve, constant current charge-discharge, AC impedance.
Embodiment three
The present embodiment comprises the following steps：
Step 1, ternary Ti3AlC2The preparation of ceramic powder；
Method according to patent ZL201310497696.9 prepares ternary layered Ti3AlC2Ceramic powder：First, according to rubbing Your ratio is Ti：Al：TiC=1.0：1.2：2.0 ratio mixes three kinds of raw materials；Secondly, three kinds of raw materials are placed in ball grinder, Using alumina balls as abrasive media, absolute ethyl alcohol is as ball-milling additive, and drum's speed of rotation is 900 revs/min, according to mass ratio For ball：Material：Ethanol=3.0：1.0：1.0 ratio, general milling 1h obtain uniform powder, and will in 40 DEG C of freeze-day with constant temperature baking ovens It is dried；Then, dried batch mixing is placed in corundum crucible, using the method for vacuum non-pressure sintering, with the liter of 8 DEG C/min Warm speed is heated to 1350 DEG C, keeps the temperature 1h, cools to room temperature with the furnace and obtain high-purity Ti3AlC2Ceramic powder.
Finally, to Ti3AlC2Ceramic powder carries out wet method high-energy ball milling 3h, and every 30 minutes once, rotating speed 400r/min, steel The mass ratio of ball and ceramic powder is 10:1, levigate powder is sieved, that is, obtains the Ti that particle diameter is less than 38 μm3AlC2Ceramic powder Body.
Step 2, two-dimensional layer Ti3C2The preparation of nano material；
Method according to patent 201410812056.7 prepares two-dimensional layer Ti3C2Nano material:Take in 5g step (1) Gained Ti3AlC2Ceramic powder is slowly immersed in 100mL 40wt% hydrofluoric acid solutions, to not after effervescent by it at room temperature Magnetic agitation 48h, rotating speed 1200r/min, with deionized water eccentric cleaning to supernatant pH value are about 5-6 by corrosion product When, then centrifuged 4 times with absolute ethyl alcohol.Black precipitate is finally dried in vacuo 24h in 40 DEG C, that is, obtains two-dimensional layer Ti3C2Nanometer Powder.
Step 3, a kind of Ti3C2-Co(OH)(CO3)0.5The preparation of nanocomposite；
First, by 291.0mg Co (NO3)2·6H2The O and Ti obtained by step (2)3C2Nano-powder 200mg is dissolved in ultrapure In water, 200mg CO (NH are successively added under magnetic stirring2)22h, which is persistently stirred, with 400mg PVP obtains mixed liquor；Secondly, will Volume fraction is transferred in the hydrothermal reaction kettle polytetrafluoroethyllining lining of 100ml for 75% mixed liquor, and the hydro-thermal assembled is anti- Kettle is answered to be warming up to 82 DEG C of insulation 8h；Then, by the product of cooled to room temperature successively with ultra-pure water and absolute ethyl alcohol respectively from Heart separation cleaning 3 times, each 4000-6000r/min centrifuge 3-5min；Finally, obtained in vacuum drying chamber after 40 DEG C of dry 24h To required Ti3C2@Co(OH)(CO3)0.5Nanocomposite.It can be seen that from the c curves of Fig. 1 in 2 θ=36 °, 42 °, 62 ° (111) are corresponded respectively to, (200), the Ti of (220) crystal face3C2Characteristic peak outside, also in 2 θ=18 °, 25 °, 34 ° correspond to PDF standard cards number are Co (OH) (CO of 48-00833)0.5(020), (111), the diffraction maximum of (221) crystal face.Show to lead to Cross hydro-thermal method and be successfully prepared Ti3C2@presomas Co (OH) (CO3)0.5Composite material.It is clear that from the c figures of Fig. 2 Ti3C2Organ shape structure, Co (OH) (CO3)0.5Pattern by nano wire becomes honeycomb and ultimately becomes nano particle to be distributed in Ti3C2Sheet surfaces and interlayer.Ti can be obtained from Fig. 33C2-Co(OH)(CO3)0.5It is demonstrated by good chemical property, CV curves Figure is preferable close to regular rectangle, symmetry；The region that cyclic curve is formed increases with the increase of sweep speed, but schemes The general shape of shape is basically unchanged, and shows good high rate performance.
Step 4, Ti3C2-Co(OH)(CO3)0.5The preparation of electrode；
First, nickel foam is cut into 1*2cm2The rectangle of size, weighs the active material i.e. step of 200mg successively Three gained Ti3C2@Co(OH)(CO3)0.5Nano-powder, the conductive acetylene of 2mg is black, the polyvinylidene fluoride of 1mg, in agate mortar Middle grinding 1-2h；Secondly, after drawing the NMP grindings uniformly of 300 μ L with liquid-transfering gun, slurry mean droplet is added in the nickel foam cut On, and by the nickel foam being added dropwise in vacuum drying chamber 60 DEG C of dry 24h；Again, by the electrode slice made under tablet press machine 15Mpa pressurizes 1min both obtains Ti3C2@Co(OH)(CO3)0.5Electrode.
Three-electrode system is finally used, with Ti3C2@Co(OH)(CO3)0.5Electrode is used as to electricity as working electrode, platinized platinum Pole, silver-colored silver chlorate is reference electrode, under the KOH electrolyte of 6M, is tested using Shanghai Chen Hua CHI660E electrochemical workstations Ti3C2@Co(OH)(CO3)0.5The chemical property of electrode, such as cyclic voltammetry curve, constant current charge-discharge, AC impedance.
Example IV
The present embodiment comprises the following steps：
Step 1, ternary Ti3AlC2The preparation of ceramic powder；
Method according to patent ZL201310497696.9 prepares ternary layered Ti3AlC2Ceramic powder：First, according to rubbing Your ratio is Ti：Al：TiC=1.0：1.2：2.0 ratio mixes three kinds of raw materials；Secondly, three kinds of raw materials are placed in ball grinder, Using alumina balls as abrasive media, absolute ethyl alcohol is as ball-milling additive, and drum's speed of rotation is 900 revs/min, according to mass ratio For ball：Material：Ethanol=3.0：1.0：1.0 ratio, general milling 1h obtain uniform powder, and will in 40 DEG C of freeze-day with constant temperature baking ovens It is dried；Then, dried batch mixing is placed in corundum crucible, using the method for vacuum non-pressure sintering, with the liter of 8 DEG C/min Warm speed is heated to 1350 DEG C, keeps the temperature 1h, cools to room temperature with the furnace and obtain high-purity Ti3AlC2Ceramic powder.
Finally, to Ti3AlC2Ceramic powder carries out wet method high-energy ball milling 3h, and every 30 minutes once, rotating speed 400r/min, steel The mass ratio of ball and ceramic powder is 10:1, levigate powder is sieved, that is, obtains the Ti that particle diameter is less than 38 μm3AlC2Ceramic powder Body.
Step 2, two-dimensional layer Ti3C2The preparation of nano material；
Method according to patent 201410812056.7 prepares two-dimensional layer Ti3C2Nano material:Take in 5g step (1) Gained Ti3AlC2Ceramic powder is slowly immersed in 100mL 40wt% hydrofluoric acid solutions, to not after effervescent by it at room temperature Magnetic agitation 48h, rotating speed 1200r/min, with deionized water eccentric cleaning to supernatant pH value are about 5-6 by corrosion product When, then centrifuged 4 times with absolute ethyl alcohol.Black precipitate is finally dried in vacuo 24h in 40 DEG C, that is, obtains two-dimensional layer Ti3C2Nanometer Powder.
Step 3, a kind of Ti3C2-Co(OH)(CO3)0.5The preparation of nanocomposite；
First, by 145.5mg Co (NO3)2·6H2The O and Ti obtained by step (2)3C2Nano-powder 200mg is dissolved in ultrapure In water, 100mg CO (NH are successively added under magnetic stirring2)22h, which is persistently stirred, with 200mg PVP obtains mixed liquor；Secondly, will Volume fraction is transferred in the hydrothermal reaction kettle polytetrafluoroethyllining lining of 100ml for 75% mixed liquor, and the hydro-thermal assembled is anti- Kettle is answered to be warming up to 82 DEG C of insulation 8h；Then, by the product of cooled to room temperature successively with ultra-pure water and absolute ethyl alcohol respectively from Heart separation cleaning 3 times, each 4000-6000r/min centrifuge 3-5min；Finally, obtained in vacuum drying chamber after 40 DEG C of dry 24h To required Ti3C2@Co(OH)(CO3)0.5Nanocomposite.It can be seen that from the d curves of Fig. 1 in 2 θ=36 °, 42 °, 62 ° (111) are corresponded respectively to, (200), the Ti of (220) crystal face3C2Characteristic peak outside, also in 2 θ=18 °, 25 °, 34 ° correspond to PDF standard cards number are Co (OH) (CO of 48-00833)0.5(020), (111), the diffraction maximum of (221) crystal face.Show to lead to Cross hydro-thermal method and be successfully prepared Ti3C2@presomas Co (OH) (CO3)0.5Composite material.From the d figures of Fig. 2 it can be seen that next, Co (OH)(CO3)0.5It is evenly distributed in Ti3C2Interlayer and measure more, do not reunite.
Step 4, Ti3C2-Co(OH)(CO3)0.5The preparation of electrode；
First, nickel foam is cut into 1*2cm2The rectangle of size, weighs the active material i.e. step of 200mg successively Three gained Ti3C2@Co(OH)(CO3)0.5Nano-powder, the conductive acetylene of 2mg is black, the polyvinylidene fluoride of 1mg, in agate mortar Middle grinding 1-2h；Secondly, after drawing the NMP grindings uniformly of 300 μ L with liquid-transfering gun, slurry mean droplet is added in the nickel foam cut On, and by the nickel foam being added dropwise in vacuum drying chamber 60 DEG C of dry 24h；Again, by the electrode slice made under tablet press machine 15Mpa pressurizes 1min both obtains Ti3C2@Co(OH)(CO3)0.5Electrode.
Three-electrode system is finally used, with Ti3C2@Co(OH)(CO3)0.5Electrode is used as to electricity as working electrode, platinized platinum Pole, silver-colored silver chlorate is reference electrode, under the KOH electrolyte of 6M, is tested using Shanghai Chen Hua CHI660E electrochemical workstations Ti3C2@Co(OH)(CO3)0.5The chemical property of electrode, such as cyclic voltammetry curve, constant current charge-discharge, AC impedance.

Claims (4)

  1. A kind of 1. Ti3C2-Co(OH)(CO3)0.5The preparation method of nanocomposite, it is characterised in that comprise the following steps：
    Step 1, prepares ternary Ti3AlC2Ceramic powder；
    Step 2, prepares two-dimensional layer Ti3C2Nano material；
    Step 3, a kind of Ti3C2-Co(OH)(CO3)0.5The preparation of nanocomposite；
    First, by 145.5-1164mg Co (NO3)2·6H2The O and two-dimensional layer Ti obtained by step (2)3C2Nano-powder 200mg It is dissolved in ultra-pure water, successively adds 100-800mg CO (NH under magnetic stirring2)20.5- is persistently stirred with 200-1600g PVP 2h obtains mixed liquor；Secondly, volume fraction is transferred to the hydrothermal reaction kettle polytetrafluoroethyllining lining of 100ml for 75% mixed liquor In, the hydrothermal reaction kettle assembled is warming up to 80-85 DEG C of insulation 6-12h；Then, by the product of cooled to room temperature successively Centrifuge cleaning 3 times respectively with ultra-pure water and absolute ethyl alcohol, each 4000-6000r/min centrifuges 3-5min；Finally, Yu Zhen In empty drying box required Ti is obtained after 40 DEG C of dry 12-24h3C2@Co(OH)(CO3)0.5Nanocomposite；
    Step 4, Ti3C2-Co(OH)(CO3)0.5The preparation of electrode；
    First, nickel foam is cut into 1*2cm2The rectangle of size, weighs the active material i.e. step 3 of 160-200mg successively Gained Ti3C2@Co(OH)(CO3)0.5Nano-powder, the conductive acetylene of 20-30mg is black, the polyvinylidene fluoride of 1-10mg, in agate 1-2h is ground in Nao mortars；Secondly, after drawing the NMP grindings uniformly of 300 μ L with liquid-transfering gun, slurry mean droplet is added in what is cut In nickel foam, and by the nickel foam being added dropwise in vacuum drying chamber 60-80 DEG C of dry 12-24h；Again, the electrode that will be made Piece 15-20Mpa pressurizes 1min under tablet press machine both obtains Ti3C2@Co(OH)(CO3)0.5Electrode.
  2. A kind of 2. Ti according to claim 13C2-Co(OH)(CO3)0.5The preparation method of nanocomposite, its feature It is, the step one prepares ternary layered Ti3AlC2Ceramic powder, is specially：First, it is Ti according to molar ratio：Al：TiC =1.0：1.2：2.0 ratio mixes three kinds of raw materials；Secondly, three kinds of raw materials are placed in ball grinder, using alumina balls as Abrasive media, absolute ethyl alcohol are 900 revs/min as ball-milling additive, drum's speed of rotation, are ball according to mass ratio：Material：Ethanol= 3.0：1.0：1.0 ratio, general milling 1h obtains uniform powder, and is baked in 40 DEG C of freeze-day with constant temperature baking ovens；Then, will Dried batch mixing is placed in corundum crucible, using the method for vacuum non-pressure sintering, is heated to the heating rate of 8 DEG C/min 1350 DEG C, 1h is kept the temperature, room temperature is cooled to the furnace and obtains high-purity Ti3AlC2Ceramic powder；Finally, to Ti3AlC2Ceramic powder carries out Wet method high-energy ball milling 3h, every 30 minutes once, rotating speed 400r/min, and the mass ratio of steel ball and ceramic powder is 10:1, will be levigate Powder sieving, that is, obtain particle diameter and be less than 38 μm of ternary Ti3AlC2Ceramic powder.
  3. A kind of 3. Ti according to claim 13C2-Co(OH)(CO3)0.5The preparation method of nanocomposite, its feature It is, the step two prepares two-dimensional layer Ti3C2Nano material, is specially：Take gained Ti in 5g step (1)3AlC2Pottery Porcelain powder is slowly immersed in 100mL 40wt% hydrofluoric acid solutions, to not after effervescent by its magnetic agitation 48h at room temperature, Rotating speed is 1200r/min, when by corrosion product with deionized water eccentric cleaning to supernatant pH value being about 5-6, then with anhydrous second Alcohol centrifuges 4 times, and black precipitate finally is dried in vacuo 24h in 40 DEG C, that is, obtains two-dimensional layer Ti3C2Nano-powder.
  4. A kind of 4. Ti according to claim 13C2-Co(OH)(CO3)0.5The preparation method of nanocomposite, its feature It is,
    Step 1, ternary Ti3AlC2The preparation of ceramic powder；
    Method according to patent ZL201310497696.9 prepares ternary layered Ti3AlC2Ceramic powder：First, according to molar ratio For Ti：Al：TiC=1.0：1.2：2.0 ratio mixes three kinds of raw materials；Secondly, three kinds of raw materials are placed in ball grinder, with oxygen It is 900 revs/min as ball-milling additive, drum's speed of rotation to change aluminium ball as abrasive media, absolute ethyl alcohol, is according to mass ratio Ball：Material：Ethanol=3.0：1.0：1.0 ratio, general milling 1h obtain uniform powder, and 40 DEG C of freeze-day with constant temperature baking ovens by its Drying；Then, dried batch mixing is placed in corundum crucible, using the method for vacuum non-pressure sintering, with the heating of 8 DEG C/min Speed is heated to 1350 DEG C, keeps the temperature 1h, cools to room temperature with the furnace and obtain high-purity Ti3AlC2Ceramic powder；
    Finally, to Ti3AlC2Ceramic powder carry out wet method high-energy ball milling 3h, every 30 minutes are once, rotating speed 400r/min, steel ball and The mass ratio of ceramic powder is 10:1, levigate powder is sieved, that is, obtains the Ti that particle diameter is less than 38 μm3AlC2Ceramic powder；
    Step 2, two-dimensional layer Ti3C2The preparation of nano material；
    Method according to patent 201410812056.7 prepares two-dimensional layer Ti3C2Nano material:Take gained in 5g step (1) Ti3AlC2Ceramic powder is slowly immersed in 100mL 40wt% hydrofluoric acid solutions, to not after effervescent by its magnetic force at room temperature 48h, rotating speed 1200r/min are stirred, when by corrosion product with deionized water eccentric cleaning to supernatant pH value being about 5-6, then Centrifuged 4 times with absolute ethyl alcohol；Black precipitate is finally dried in vacuo 24h in 40 DEG C, that is, obtains two-dimensional layer Ti3C2Nano-powder；
    Step 3, a kind of Ti3C2-Co(OH)(CO3)0.5The preparation of nanocomposite；
    First, by 291.0mg Co (NO3)2·6H2The O and Ti obtained by step (2)3C2Nano-powder 200mg is dissolved in ultra-pure water, 200mg CO (NH are successively added under magnetic stirring2)22h, which is persistently stirred, with 400mg PVP obtains mixed liquor；Secondly, by volume Fraction is transferred in the hydrothermal reaction kettle polytetrafluoroethyllining lining of 100ml for 75% mixed liquor, the hydrothermal reaction kettle that will be assembled It is warming up to 82 DEG C of insulation 8h；Then, the product of cooled to room temperature is centrifuged point respectively with ultra-pure water and absolute ethyl alcohol successively 3 times from cleaning, each 4000-6000r/min centrifuges 3-5min；Finally, in vacuum drying chamber institute is obtained after 40 DEG C of dry 24h Need Ti3C2@Co(OH)(CO3)0.5Nanocomposite；
    Step 4, Ti3C2-Co(OH)(CO3)0.5The preparation of electrode；
    First, nickel foam is cut into 1*2cm2The rectangle of size, weighs obtained by the active material i.e. step 3 of 200mg successively Ti3C2@Co(OH)(CO3)0.5Nano-powder, the conductive acetylene of 2mg is black, and the polyvinylidene fluoride of 1mg, grinds in agate mortar 1-2h；Secondly, after drawing the NMP grindings uniformly of 300 μ L with liquid-transfering gun, slurry mean droplet is added in the nickel foam cut, and By the nickel foam being added dropwise in vacuum drying chamber 60 DEG C of dry 24h；Again, by the electrode slice made under tablet press machine 15Mpa Pressurize 1min both obtains Ti3C2@Co(OH)(CO3)0.5Electrode.
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