CN106563479B - A kind of two dimension carbide supported rare earth fluoride nano powder, preparation method and applications - Google Patents
A kind of two dimension carbide supported rare earth fluoride nano powder, preparation method and applications Download PDFInfo
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Abstract
A kind of two dimension carbide supported rare earth fluoride nano raw powder's production technology, steps are as follows: (1) MAX phase ceramics powder is immersed in hydrochloric acid solution dissolved with lithium fluoride, is stirred, centrifuge separation, it is successively cleaned with deionized water and ethyl alcohol, obtained solid powder is two-dimentional carbide after drying；(2) two-dimentional carbide is added in rare earth nitrate aqueous solution, places 8-24h after stirring evenly, is freeze-dried to obtain two-dimentional carbide supported rare earth nitrate composite precursor；Wherein, the concentration of rare earth nitrate aqueous solution is 0.1-1g/mL, and 0.5 ~ 1g of two-dimentional carbide is added in every 1mL rare earth nitrate aqueous solution；(3) under the protection of argon gas, nitrogen or helium, 400-600 DEG C of roasting 0.5-2h is washed, is drying to obtain two-dimentional carbide supported rare earth fluoride nano powder.
Description
Technical field
The invention belongs to nanocomposite preparation fields, and in particular to it is a kind of two dimension carbide supported rare earth fluoride receive
Rice flour body, preparation method and applications.
Background technique
Mxene is a kind of New Two Dimensional crystalline transition metal carbides, has structure similar with graphene, by using
Element A etching in presoma MAX phase is prepared the mixed solution of villiaumite and hydrochloric acid, is the ternary layered compound of MAX phase
General name, wherein M is early stage transition metal element, and A is third and fourth major element, and X is carbon or nitrogen；Up to the present, have 70
A variety of MAX phases are reported, and the MXene being successfully prepared is mainly include the following types: Ti3C2, Ti2C, Mo2C, (Ti0.5,
Nb0.5)2C, Ti3CN, Sc2C, Ta4C3, Nb2C, V2C and Nb4C3.Have by MXene prepared by liquid phase relatively high
Specific surface area and lamellar structure arranged in a uniform, excellent thermal stability, electricity and optical characteristics, so that MXene is being catalyzed
Field, adsorbent material field etc. are well used.Hydrogen is hydrogen energy source neck with storage as a kind of clean energy resource, preparation
The research hotspot in domain, combustion product is pollution-free, can be repeatedly circulated.Lithium ion battery is excellent as energy storage device
Different memory capacity, cyclical stability and higher cycle rate depend on the electrode material of lithium battery.It is therefore desirable to find
New approach and material improve the performance of hydrogen output and lithium ion battery.
The work studied in the prior art is mainly MXene one-component and load oxidate nano composite material and metal list
Absorption, lithium electricity and the supercapacitor of matter etc. performance, seldom study two-dimensional carbide nanometer material are received with rare earth fluoride
The load of rice grain.
Summary of the invention
The object of the present invention is to provide a kind of two-dimentional carbide supported rare earth fluoride nano powder, preparation method and its answer
With.
Based on above-mentioned purpose, the present invention is adopted the following technical scheme that:
A kind of two dimension carbide MXene supported rare earth fluoride nano raw powder's production technology, includes the following steps:
(1) MAX phase ceramics powder is immersed in the hydrochloric acid solution dissolved with villiaumite, is stirred, centrifuge separation is successively spent
Ionized water and ethyl alcohol cleaning, obtained solid powder is two-dimentional carbide (i.e. MXene) after drying；
(2) two-dimentional carbide is added in rare earth nitrate aqueous solution, places 8-24h after stirring evenly, is freeze-dried two-dimentional
Carbide supported rare earth nitrate composite precursor；Wherein, the concentration of rare earth nitrate aqueous solution is 0.1-1g/mL, and every 1mL is dilute
0.5 ~ 1g of two-dimentional carbide is added in native nitrate aqueous solution；
(3) under the protection of argon gas, nitrogen or helium, 400-600 DEG C of roasting 0.5-2h is washed, is drying to obtain Two-dimensional Carbon
Compound supported rare earth fluoride nano powder.
Further, two dimension carbide MXene described in step (1) is Ti3C2、Ti2C or V2C。
Rare earth nitrades are lanthanum nitrate, cerous nitrate, yttrium nitrate, dysprosium nitrate, erbium nitrate, neodymium nitrate, nitric acid in step (1)
At least one of samarium, gadolinium nitrate and terbium nitrate.
In step (1) freeze-drying refer to more than vacuum degree 20Pa, -20 DEG C of temperature or less dry at least 12h.
Using two-dimentional carbide supported rare earth fluoride nano powder obtained by above-mentioned preparation method.
Application of the above-mentioned two dimension carbide supported rare earth fluoride nano powder in terms of being catalyzed hydrogen storage.
Application of the above-mentioned two dimension carbide supported rare earth fluoride nano powder in terms of lithium battery.
Two dimension carbide supported rare earth fluoride nano raw powder's production technology of the invention does not need to add any catalyst,
And rare earth fluoride load capacity is adjustable, reaction can carry out at different temperatures, and reaction condition is mild, and MXene is evenly distributed orderly
Lamellar structure, provide preferable carrier for rare-earth fluoride nano particle.Present invention process method is simple, it is low in cost,
Without special process equipment, convenience and high-efficiency, rare-earth fluoride nano particle is realized in the surface two-dimentional carbide MXene and interlayer
Uniform load, this method can load on a variety of rare-earth fluoride nano particles to MXene, prepared two-dimentional carbide
MXene supported rare earth fluoride nano powder has a good application prospect in fields such as hydrogen storage, lithium electricity.
Detailed description of the invention
Fig. 1 is two-dimentional carbide load C eF prepared by the embodiment of the present invention 13The X ray diffracting spectrum of nano-powder；
Fig. 2 is two-dimentional carbide load C eF prepared by the embodiment of the present invention 13The field emission scanning electron microscope of nano-powder shines
Piece；
Fig. 3 is that two-dimentional carbide prepared by the embodiment of the present invention 2 loads YF3The X ray diffracting spectrum of nano-powder；
Fig. 4 is that two-dimentional carbide prepared by the embodiment of the present invention 2 loads YF3The field emission scanning electron microscope of nano-powder shines
Piece；
Fig. 5 is two-dimentional carbide load C eF prepared by the embodiment of the present invention 13The hydrogen storage property test result of nano-powder；
Fig. 6 is two-dimentional carbide load C eF prepared by the embodiment of the present invention 13The lithium electric performance test result of nano-powder.
Specific embodiment
Below in conjunction with specific embodiment, further details of the technical solution of the present invention, but protection model of the invention
It encloses and is not limited thereto.
Embodiment 1
A kind of two dimension carbide Ti3C2Supported rare earth fluoride CeF3The preparation method of nano-powder, including walk as follows
It is rapid:
(1) by 5g MAX phase Ti3AlC2Powder is immersed in the hydrochloric acid solution of the 100mL 6M dissolved with 5g lithium fluoride, and 60
Magnetic agitation 48h at a temperature of DEG C, centrifuge separation precipitating clean to close to neutral through deionized water and use washes of absolute alcohol three again
Time, 12h is dried in vacuo at a temperature of 80 DEG C will be deposited in, obtained solid powder is two-dimentional carbide Ti3C2；
(2) it weighs 0.31g cerous nitrate to be dissolved in 1mL deionized water, room temperature stirs evenly, and obtains cerous nitrate aqueous solution；By 1g bis-
Tie up carbide Ti3C2Solid powder ultrasound 0.5h is dispersed in above-mentioned cerous nitrate aqueous solution, is placed 12 hours after mixing evenly；It
Afterwards in the case where vacuum degree is 20Pa, -20 DEG C of dry 12h obtain Ti3C2Load cerous nitrate composite precursor；
(3) in an ar atmosphere, it roasts 1 hour for 450 DEG C, after reaction, products therefrom is successively washed with deionized
Three times, three times, 80 DEG C of vacuum dry 12h are to get two-dimentional carbide Ti for dehydrated alcohol washing3C2Load C eF3Nano-powder, product
It is its X ray diffracting spectrum labeled as A-1, Fig. 1, it will be apparent that CeF occur3Diffraction maximum；Fig. 2 is its field emission scanning electron microscope
Photo, it can be seen that Ti3C2Area load CeF3Nano particle diameter is 20-400nm.
Embodiment 2
A kind of two dimension carbide V2C supported rare earth fluoride YF3The preparation method of nano-powder, includes the following steps:
(1) by 5g MAX phase V2AlC powder is immersed in the hydrochloric acid solution of the 100mL 6M dissolved with 5g sodium fluoride, and 90 DEG C
At a temperature of magnetic agitation 72h, centrifuge separation precipitating, through deionized water clean to close to neutral again using washes of absolute alcohol three
Time, 12h is dried in vacuo at a temperature of 80 DEG C will be deposited in, obtained solid powder is two-dimentional carbide V2C；
(2) it weighs 0.15g yttrium nitrate to be dissolved in 1mL deionized water, room temperature stirs evenly, and obtains yttrium nitrate aqueous solution；By 1g bis-
Tie up carbide V2C solid powder ultrasound 0.5h is dispersed in above-mentioned yttrium nitrate aqueous solution, is placed 12 hours after mixing evenly；Later
In the case where vacuum degree is 25Pa, -25 DEG C of dry 12h obtain V2C loads yttrium nitrate composite precursor；
(3) in an ar atmosphere, it roasts 1 hour for 450 DEG C, after reaction, products therefrom is successively washed with deionized
Three times, three times, 80 DEG C of vacuum dry 12h are to get two-dimentional carbide V for dehydrated alcohol washing2C loads YF3Nano-powder, product mark
It is denoted as A-2, Fig. 3 is its X ray diffracting spectrum, it will be apparent that YF occurs3Diffraction maximum；Fig. 4 is its field emission scanning electron microscope photograph
Piece, it can be seen that V2C Surface loads YF3Nano particle diameter is 20-400nm.
Embodiment 3
A kind of two dimension carbide Ti3C2Supported rare earth fluoride LaF3The preparation method of nano-powder, including walk as follows
It is rapid:
(1) by 5g MAX phase Ti3AlC2Powder is immersed in the hydrochloric acid solution of the 100mL 6M dissolved with 5g lithium fluoride, and 60
Magnetic agitation 48h at a temperature of DEG C, centrifuge separation precipitating clean to close to neutral through deionized water and use washes of absolute alcohol three again
Time, it is dried in vacuo at a temperature of 80 DEG C will be deposited in for 24 hours, obtained solid powder is two-dimentional carbide Ti3C2；
(2) it weighs 0.31g lanthanum nitrate to be dissolved in 1mL deionized water, room temperature stirs evenly, and obtains lanthanum nitrate aqueous solution；By 0.5g
Two-dimentional carbide Ti3C2Solid powder ultrasound 1h is dispersed in above-mentioned lanthanum nitrate aqueous solution, is placed 24 hours after mixing evenly；It
Afterwards in the case where vacuum degree is 30Pa, -20 DEG C of dryings obtain Ti for 24 hours3C2Load lanthanum nitrate composite precursor；
(3) in an ar atmosphere, it roasts 1 hour for 600 DEG C, after reaction, products therefrom is successively washed with deionized
Three times, three times, 100 DEG C of vacuum dry 12h are to get two-dimentional carbide Ti for dehydrated alcohol washing3C2Load LaF3Nano-powder.
Embodiment 4
A kind of two dimension carbide V2C supported rare earth fluoride TbF3The preparation method of nano-powder, includes the following steps:
(1) by 5g MAX phase V2AlC powder is immersed in the hydrochloric acid solution of the 100mL 6M dissolved with 5g sodium fluoride, and 90 DEG C
At a temperature of magnetic agitation 72h, centrifuge separation precipitating, through deionized water clean to close to neutral again using washes of absolute alcohol three
Time, 12h is dried in vacuo at a temperature of 100 DEG C will be deposited in, obtained solid powder is two-dimentional carbide V2C；
(2) it weighs 0.31g terbium nitrate to be dissolved in 1mL deionized water, room temperature stirs evenly, and obtains terbium nitrate aqueous solution；By 1g bis-
Tie up carbide V2C solid powder ultrasound 40min is dispersed in above-mentioned terbium nitrate aqueous solution, is placed 8 hours after mixing evenly；Later
In the case where vacuum degree is 25Pa, -40 DEG C of dry 12h obtain V2C loads terbium nitrate composite precursor；
(3) in an ar atmosphere, it roasts 1 hour for 500 DEG C, after reaction, products therefrom is successively washed with deionized
Three times, three times, 80 DEG C of vacuum dry 18h are to get two-dimentional carbide V for dehydrated alcohol washing2C loads TbF3Nano-powder.
Embodiment 5
A kind of two dimension carbide V2C supported rare earth fluoride NdF3The preparation method of nano-powder, includes the following steps:
(1) by 5g MAX phase V2AlC powder is immersed in the hydrochloric acid solution of the 100mL 6M dissolved with 5g sodium fluoride, and 90 DEG C
At a temperature of magnetic agitation 72h, centrifuge separation precipitating, through deionized water clean to close to neutral again using washes of absolute alcohol three
Time, 12h is dried in vacuo at a temperature of 80 DEG C will be deposited in, obtained solid powder is two-dimentional carbide V2C；
(2) it weighs 0.31g neodymium nitrate to be dissolved in 1mL deionized water, room temperature stirs evenly, and obtains aqueous neodymium nitrate；By 0.5g
Two-dimentional carbide V2C solid powder ultrasound 0.5h is dispersed in above-mentioned aqueous neodymium nitrate, is placed 12 hours after mixing evenly；It
Afterwards in the case where vacuum degree is 35Pa, -30 DEG C of dry 12h obtain V2C loads neodymium nitrate composite precursor；
(3) in an ar atmosphere, it roasts 1 hour for 550 DEG C, after reaction, products therefrom is successively washed with deionized
Three times, three times, 90 DEG C of vacuum dry 16h are to get two-dimentional carbide V for dehydrated alcohol washing2C loads NdF3Nano-powder.
Application of the two-dimentional carbide supported rare earth fluoride nano powder in terms of being catalyzed hydrogen storage
The NaAlH of 0.9g is weighed respectively4With Two-dimensional Carbon made from two-dimentional carbide prepared by 0.1g or 0.1g embodiment 1
Compound Ti3C2Load C eF3Nano-powder, and 12h is ground in a planetary ball mill, obtained mixed powder is respectively at 100 DEG C
Lower its constant temperature hydrogen discharging performance of test.Test results are shown in figure 5, two-dimentional carbide Ti3C2Load C eF3 nano-powder is at 100 DEG C
At a temperature of be catalyzed the rate of NaAlH4 hydrogen release and significantly improve, the i.e. H of releasable 3.10wt% in 3h2, 6h can discharge 3.33wt%
H2；In contrast, two-dimentional carbides catalytic NaAlH4Hydrogen release is obviously poor, and the hydrogen desorption capacity of 6h only has 2.83wt%, and hydrogen release speed
Rate is slower.By comparison, it was found that MXene supported rare earth fluoride nano powder has more excellent catalytic than pure MXene
Can, it is remarkably improved NaAlH4Hydrogen discharging rate, improve hydrogen desorption capacity, so as to improve NaAlH4Hydrogen storage property.In addition, to implementation
The nano-powder that example 2 to 5 obtains also has carried out the test in terms of catalysis hydrogen storage under similarity condition, as a result proves embodiment 2 to 5
Obtained nano-powder catalysis NaAlH4Hydrogen discharging rate and two-dimentional carbide Ti3C2Load C eF3Nano-powder is suitable, therefore,
The nano-powder that embodiment 2 to 5 obtains also has a good application prospect in terms of being catalyzed hydrogen storage.
Application of the two-dimentional carbide supported rare earth fluoride nano powder in terms of lithium battery
Weigh two dimension carbide Ti made from embodiment 13C2Load C eF3Nano-powder, acetylene black and polytetrafluoroethylene (PTFE) are pressed
The quality of 0.3457g:0.0432g:0.0432g is more uniform than mixed grinding, and about 35 drop N-Methyl pyrrolidones are added, stir into
Uniform slurry is coated on copper foil, 110 DEG C of vacuum drying 12h, and it is 14mm disk as cathode, gold that copper foil, which is cut into diameter,
Belong to lithium as anode, (model: electrolyte 14712 is purchased from the limited public affairs of Dongguan City China fir China fir battery material to lithium-ion battery electrolytes
Department) it is used as electrolyte, button cell is assembled into glove box, then carry out constant current charge-discharge test.Test result such as Fig. 6 institute
Show, MXene load C eF3Nano-powder is 305.75mAh/g as the discharge capacity for the first time of battery electrode, and MXene is as electricity
The discharge capacity for the first time of pond electrode is 221.0mAh/g, i.e., the lithium battery after MXene supported rare earth fluoride nano grain can be obvious
There is higher discharge capacity than pure MXene.In addition, also being carried out under similarity condition to the nano-powder that embodiment 2 to 5 obtains
Constant current charge-discharge test, as a result prove the nano-powder that embodiment 2 to 5 obtains discharge capacity and two-dimentional carbide Ti3C2It is negative
Carry CeF3Nano-powder is suitable, and therefore, the nano-powder that embodiment 2 to 5 obtains also has good application in terms of lithium battery
Prospect.
Finally, it is noted that be not intended to restrict the invention the foregoing is merely preferred embodiment of the invention, it is right
For those skilled in the art, the invention may be variously modified and varied.All within the spirits and principles of the present invention,
Any modification, equivalent substitution and improvement retouching done etc., should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of two dimension carbide supported rare earth fluoride nano raw powder's production technology, which comprises the steps of:
(1) MAX phase ceramics powder is immersed in the hydrochloric acid solution dissolved with lithium fluoride, stir, centrifuge separation, successively spend from
Sub- water and ethyl alcohol cleaning, obtained solid powder is two-dimentional carbide after drying；
(2) two-dimentional carbide is added in rare earth nitrate aqueous solution, places 8-24h after stirring evenly, is freeze-dried to obtain two-dimentional carbonization
Object supported rare earth nitrate composite precursor；Wherein, the concentration of rare earth nitrate aqueous solution is 0.1-1g/mL, every 1mL rare earth nitre
0.5 ~ 1g of two-dimentional carbide is added in acid salt aqueous solution；
(3) under the protection of argon gas, nitrogen or helium, 400-600 DEG C of roasting 0.5-2h is washed, is drying to obtain two-dimentional carbide
Supported rare earth fluoride nano powder.
2. two dimension carbide supported rare earth fluoride nano raw powder's production technology according to claim 1, feature exist
In two dimension carbide described in step (1) is Ti3C2、Ti2C or V2C。
3. two dimension carbide supported rare earth fluoride nano raw powder's production technology according to claim 1, feature exist
In rare earth nitrades are lanthanum nitrate, cerous nitrate, yttrium nitrate, dysprosium nitrate, erbium nitrate, neodymium nitrate, samaric nitrate, nitric acid in step (1)
At least one of gadolinium and terbium nitrate.
4. two dimension carbide supported rare earth fluoride nano raw powder's production technology according to claim 3, feature exist
In rare earth nitrades are at least one of cerous nitrate and yttrium nitrate in step (1).
5. two dimension carbide supported rare earth fluoride nano raw powder's production technology according to claim 1, feature exist
In, step (1) freeze-drying refer to more than vacuum degree 20Pa, -20 DEG C of temperature or less dry at least 12h.
6. using two dimension carbide supported rare earth fluoride nano powder made from any preparation method of claim 1 to 5
Body.
7. application of the two dimension carbide supported rare earth fluoride nano powder as claimed in claim 6 in terms of catalyzing manufacturing of hydrogen.
8. application of the two dimension carbide supported rare earth fluoride nano powder as claimed in claim 6 in terms of lithium battery.
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