CN106563479A - Two-dimensional carbide-supported rare earth fluoride nanometer powder, preparation method and applications thereof - Google Patents
Two-dimensional carbide-supported rare earth fluoride nanometer powder, preparation method and applications thereof Download PDFInfo
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- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention provides a two-dimensional carbide-supported rare earth fluoride nanometer powder preparation method, which comprises: (1) immersing MAX-phase ceramic powder in a hydrochloric acid solution with lithium fluoride dissolved inside, stirring, carrying out centrifugal separation, washing sequentially with deionized water and ethanol, and drying to obtain solid powder, ie., a two-dimensional carbide; (2) adding the two-dimensional carbide to a rare earth nitrate aqueous solution, uniformly stirring, placing for 8-24 h, and carrying out freeze-drying to obtain a two-dimensional carbide-supported rare earth nitrate composite precursor, wherein the concentration of the rare earth nitrate aqueous solution is 0.1-1 g/mL, and 0.5-1 g of the two-dimensional carbide is added to per 1 mL of the rare earth nitrate aqueous solution; and (3) under the protection of argon, nitrogen or helium, calcining for 0.5-2 h at a temperature of 400-600 DEG C, washing, and drying to obtain the two-dimensional carbide-supported rare earth fluoride nanometer powder.
Description
Technical field
The invention belongs to nano composite material preparation field, and in particular to a kind of two-dimentional carbide supported rare earth fluoride is received
Rice flour body, preparation method and applications.
Background technology
Mxene is a kind of New Two Dimensional crystalline transition metal carbides, with the structure similar with Graphene, by adopting
The mixed solution of villiaumite and hydrochloric acid prepares the element A etching in presoma MAX phases, is the ternary layered compound of MAX phases
General name, wherein M is early stage transition metal, and A is third and fourth major element, and X is carbon or nitrogen；Up to the present, existing 70
Various MAX phases are reported, and the MXene for successfully preparing mainly has following several：Ti3C2, Ti2C, Mo2C, (Ti0.5,
Nb0.5)2C, Ti3CN, Sc2C, Ta4C3, Nb2C, V2C and Nb4C3.The MXene prepared by liquid phase has of a relatively high
Specific surface area, and lamellar structure arranged in a uniform, excellent heat stability, electricity and optical characteristics so that MXene is in catalysis
Field, adsorbing material field etc. are well used.Used as a kind of clean energy resource, it is hydrogen energy source neck that it is prepared with storage to hydrogen
The study hotspot in domain, combustion product is pollution-free, can be repeatedly circulated.Lithium ion battery is used as energy storing device, and its is excellent
Different memory capacity, cyclical stability, and higher cycle rate depend on the electrode material of lithium battery.It is therefore desirable to finding
New approach and material improves the performance of hydrogen output and lithium ion battery.
The work studied in prior art is mainly MXene one-components and load oxidate nano composite and metal list
The aspect performances such as the absorption of matter, lithium electricity and ultracapacitor, little study two-dimensional carbide nanometer material is received with rare earth fluoride
The load of rice grain.
The content of the invention
It is an object of the invention to provide a kind of two-dimentional carbide supported rare earth fluoride nano powder body, preparation method and its should
With.
Based on above-mentioned purpose, the present invention is adopted the following technical scheme that：
A kind of two-dimentional carbide MXene supported rare earths fluoride nano raw powder's production technology, comprises the steps：
（1）MAX phase ceramics powder is immersed in the hydrochloric acid solution for being dissolved with villiaumite, is stirred, deionization is used successively in centrifugation
Water and ethanol purge, gained pressed powder is two-dimentional carbide after being dried（That is MXene）；
（2）Two-dimentional carbide is added in rare earth nitrate aqueous solution, 8-24h is placed after stirring evenly, lyophilization obtains two-dimentional carbonization
Thing supported rare earth nitrate composite precursor；Wherein, the concentration of rare earth nitrate aqueous solution is 0.1-1g/mL, per 1mL rare earth nitre
0.5 ~ 1g of two-dimentional carbide is added in acid salt aqueous solution；
（3）Under the protection of argon, 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 body.
Further, step（1）Described in two-dimentional carbide MXene be Ti3C2、Ti2C or V2C。
Step（1）Middle rare earth nitrate is Lanthanum (III) nitrate, cerous nitrate, Yttrium trinitrate, Dysprosium trinitrate, Erbium trinitrate, neodymium nitrate, nitric acid
At least one in samarium, Gadolinium trinitrate and Terbium nitrate (Tb(NO3)3).
Step（1）Middle lyophilization is referred to more than vacuum 20Pa, at least 12h is dried below -20 DEG C of temperature.
Using the two-dimentional carbide supported rare earth fluoride nano powder body obtained by above-mentioned preparation method.
Application of the above-mentioned two-dimentional carbide supported rare earth fluoride nano powder body in terms of catalysis hydrogen storage.
Application of the above-mentioned two-dimentional carbide supported rare earth fluoride nano powder body in terms of lithium battery.
Two dimension carbide supported rare earth fluoride nano raw powder's production technology of the invention need not add any catalyst,
And rare earth fluoride load capacity is adjustable, reaction can be carried out at different temperatures, and reaction condition is gentle, and MXene is evenly distributed in order
Lamellar structure, provide preferable carrier for rare-earth fluoride nano granule.Present invention process method is simple, with low cost,
Without the need for special process equipment, convenience and high-efficiency, rare-earth fluoride nano granule is realized in two-dimentional carbide MXene surfaces and interlayer
Uniform load, the method can load various rare-earth fluoride nano granules on MXene, prepared two-dimentional carbide
MXene supported rare earth fluoride nano powder body has a good application prospect in fields such as hydrogen storage, lithium electricity.
Description of the drawings
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 photo of nano-powder；
Fig. 3 is two-dimentional carbide load YF prepared by the embodiment of the present invention 23The X ray diffracting spectrum of nano-powder；
Fig. 4 is two-dimentional carbide load YF prepared by the embodiment of the present invention 23The field emission scanning electron microscope photo of nano-powder；
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
Technical scheme is described in further details below in conjunction with specific embodiment, but the protection model of the present invention
Enclose and be not limited thereto.
Embodiment 1
A kind of two-dimentional carbide Ti3C2Supported rare earth fluoride CeF3Its preparation method of nano-powder, comprises the steps：
（1）By 5g MAX phases Ti3AlC2Powder is immersed in the hydrochloric acid solution of the 100mL 6M for being dissolved with 5g lithium fluoride, 60 DEG C of temperature
Lower magnetic agitation 48h of degree, centrifugation precipitation, Jing deionized waters are cleaned to close neutral again using washes of absolute alcohol three times,
12h will be vacuum dried at a temperature of 80 DEG C will be deposited in, gained pressed powder is two-dimentional carbide Ti3C2；
（2）Weigh 0.31g cerous nitrates to be dissolved in 1mL deionized waters, room temperature is stirred evenly, obtain cerous nitrate aqueous solution；By 1g Two-dimensional Carbons
Compound Ti3C2Pressed powder ultrasound 0.5h is dispersed in above-mentioned cerous nitrate aqueous solution, is placed 12 hours after stirring；Exist afterwards
Vacuum is that -20 DEG C are dried 12h and obtain Ti under 20Pa3C2Load cerous nitrate composite precursor；
（3）In an ar atmosphere, 450 DEG C of roastings 1 hour, after reaction terminates, products therefrom is washed with deionized successively three times,
Absolute ethanol washing three times, 80 DEG C of vacuum is dried 12h, obtains final product two-dimentional carbide Ti3C2Load C eF3Nano-powder, Product Labeling
For A-1, Fig. 1 is its X ray diffracting spectrum, it will be apparent that occur in that CeF3Diffraction maximum；Fig. 2 shines for its field emission scanning electron microscope
Piece, it can be seen that Ti3C2Area load CeF3Nano particle diameter is 20-400nm.
Embodiment 2
A kind of two-dimentional carbide V2C supported rare earth fluoride YF3Its preparation method of nano-powder, comprises the steps：
（1）By 5g MAX phases V2AlC powder is immersed in the hydrochloric acid solution of the 100mL 6M for being dissolved with 5g sodium fluoride, 90 DEG C of temperature
Lower magnetic agitation 72h, centrifugation precipitation, Jing deionized waters are cleaned to close neutral again using washes of absolute alcohol three times, will
12h is vacuum dried at a temperature of being deposited in 80 DEG C, gained pressed powder is two-dimentional carbide V2C；
（2）Weigh 0.15g Yttrium trinitrates to be dissolved in 1mL deionized waters, room temperature is stirred evenly, and obtains yttrium nitrate aqueous solution；By 1g Two-dimensional Carbons
Compound V2C pressed powders ultrasound 0.5h is dispersed in above-mentioned yttrium nitrate aqueous solution, is placed 12 hours after stirring；Afterwards true
Reciprocal of duty cycle is that -25 DEG C are dried 12h and obtain V under 25Pa2C loads Yttrium trinitrate composite precursor；
（3）In an ar atmosphere, 450 DEG C of roastings 1 hour, after reaction terminates, products therefrom are washed with deionized successively three times,
Absolute ethanol washing three times, 80 DEG C of vacuum is dried 12h, obtains final product two-dimentional carbide V2C loads YF3Nano-powder, Product Labeling is A-
2, Fig. 3 is its X ray diffracting spectrum, it will be apparent that occur in that YF3Diffraction maximum；Fig. 4 is its field emission scanning electron microscope photo, can be with
Find out, V2C Surface loads YF3Nano particle diameter is 20-400nm.
Embodiment 3
A kind of two-dimentional carbide Ti3C2Supported rare earth fluoride LaF3Its preparation method of nano-powder, comprises the steps：
（1）By 5g MAX phases Ti3AlC2Powder is immersed in the hydrochloric acid solution of the 100mL 6M for being dissolved with 5g lithium fluoride, 60 DEG C of temperature
Lower magnetic agitation 48h of degree, centrifugation precipitation, Jing deionized waters are cleaned to close neutral again using washes of absolute alcohol three times,
24h will be vacuum dried at a temperature of 80 DEG C will be deposited in, gained pressed powder is two-dimentional carbide Ti3C2；
（2）Weigh 0.31g Lanthanum (III) nitrates to be dissolved in 1mL deionized waters, room temperature is stirred evenly, and obtains lanthanum nitrate aqueous solution；0.5g is two-dimentional
Carbide Ti3C2Pressed powder ultrasound 1h is dispersed in above-mentioned lanthanum nitrate aqueous solution, is placed 24 hours after stirring；Exist afterwards
Vacuum is that -20 DEG C are dried 24h and obtain Ti under 30Pa3C2Load Lanthanum (III) nitrate composite precursor；
（3）In an ar atmosphere, 600 DEG C of roastings 1 hour, after reaction terminates, products therefrom is washed with deionized successively three times,
Absolute ethanol washing three times, 100 DEG C of vacuum is dried 12h, obtains final product two-dimentional carbide Ti3C2Load LaF3Nano-powder.
Embodiment 4
A kind of two-dimentional carbide V2C supported rare earth fluoride TbF3Its preparation method of nano-powder, comprises the steps：
（1）By 5g MAX phases V2AlC powder is immersed in the hydrochloric acid solution of the 100mL 6M for being dissolved with 5g sodium fluoride, 90 DEG C of temperature
Lower magnetic agitation 72h, centrifugation precipitation, Jing deionized waters are cleaned to close neutral again using washes of absolute alcohol three times, will
12h is vacuum dried at a temperature of being deposited in 100 DEG C, gained pressed powder is two-dimentional carbide V2C；
（2）Weigh 0.31g Terbium nitrate (Tb(NO3)3)s to be dissolved in 1mL deionized waters, room temperature is stirred evenly, obtain Terbium nitrate (Tb(NO3)3) aqueous solution；By 1g Two-dimensional Carbons
Compound V2C pressed powders ultrasound 40min is dispersed in above-mentioned Terbium nitrate (Tb(NO3)3) aqueous solution, is placed 8 hours after stirring；Afterwards true
Reciprocal of duty cycle is that -40 DEG C are dried 12h and obtain V under 25Pa2C loads Terbium nitrate (Tb(NO3)3) composite precursor；
（3）In an ar atmosphere, 500 DEG C of roastings 1 hour, after reaction terminates, products therefrom are washed with deionized successively three times,
Absolute ethanol washing three times, 80 DEG C of vacuum is dried 18h, obtains final product two-dimentional carbide V2C loads TbF3Nano-powder.
Embodiment 5
A kind of two-dimentional carbide V2C supported rare earth fluoride NdF3Its preparation method of nano-powder, comprises the steps：
（1）By 5g MAX phases V2AlC powder is immersed in the hydrochloric acid solution of the 100mL 6M for being dissolved with 5g sodium fluoride, 90 DEG C of temperature
Lower magnetic agitation 72h, centrifugation precipitation, Jing deionized waters are cleaned to close neutral again using washes of absolute alcohol three times, will
12h is vacuum dried at a temperature of being deposited in 80 DEG C, gained pressed powder is two-dimentional carbide V2C；
（2）Weigh 0.31g neodymium nitrates to be dissolved in 1mL deionized waters, room temperature is stirred evenly, and obtains aqueous neodymium nitrate；0.5g is two-dimentional
Carbide V2C pressed powders ultrasound 0.5h is dispersed in above-mentioned aqueous neodymium nitrate, is placed 12 hours after stirring；Exist afterwards
Vacuum is that -30 DEG C are dried 12h and obtain V under 35Pa2C loads neodymium nitrate composite precursor；
（3）In an ar atmosphere, 550 DEG C of roastings 1 hour, after reaction terminates, products therefrom are washed with deionized successively three times,
Absolute ethanol washing three times, 90 DEG C of vacuum is dried 16h, obtains final product two-dimentional carbide V2C loads NdF3Nano-powder.
Application of the two-dimentional carbide supported rare earth fluoride nano powder body in terms of catalysis hydrogen storage
The NaAlH of 0.9g is weighed respectively4With two-dimentional carbide obtained in the two-dimentional carbide or 0.1g embodiments 1 prepared by 0.1g
Ti3C2Load C eF3Nano-powder, and in planetary grinding in ball grinder 12h, the mixed powder for obtaining is surveyed respectively at 100 DEG C
Try its constant temperature hydrogen discharging performance.Test result is as shown in figure 5, two-dimentional carbide Ti3C2Load C eF3 nano-powder is in 100 DEG C of temperature
The speed that lower catalysis NaAlH4 puts hydrogen is significantly improved, the i.e. H of releasable 3.10wt% in 3h2, 6h can discharge the H of 3.33wt%2；
By contrast, two-dimentional carbides catalytic NaAlH4Put that hydrogen is substantially poor, the hydrogen desorption capacity of 6h only has 2.83wt%, and hydrogen discharging rate compared with
Slowly.Found by contrasting, MXene supported rare earth fluoride nano powder body has more excellent catalytic performance than pure MXene, can
Significantly improve NaAlH4Hydrogen discharging rate, improve hydrogen desorption capacity, so as to improve NaAlH4Hydrogen storage property.Additionally, to embodiment 2 to 5
The nano-powder for obtaining has been also carried out being catalyzed the test in terms of hydrogen storage under similarity condition, as a result proves what embodiment 2 to 5 was obtained
Nano-powder is catalyzed NaAlH4Hydrogen discharging rate and two-dimentional carbide Ti3C2Load C eF3Nano-powder is suitable, therefore, embodiment 2
Also have a good application prospect in terms of catalysis hydrogen storage to 5 nano-powders for obtaining.
Application of the two-dimentional carbide supported rare earth fluoride nano powder body in terms of lithium battery
Weigh two-dimentional carbide Ti obtained in embodiment 13C2Load C eF3Nano-powder, acetylene black and politef are pressed
0.3457g：0.0432g：The quality of 0.0432g is more uniform than mixed grinding, adds about 35 to drip N-Methyl pyrrolidone, stirs into
Uniform slurry, is coated on Copper Foil, 110 DEG C of vacuum drying 12h, and Copper Foil is cut into a diameter of 14mm disks as negative pole, gold
Category lithium is used as positive pole, lithium-ion battery electrolytes（Model：Electrolyte 14712, purchased from the limited public affairs of Dongguan City China fir China fir battery material
Department）As electrolyte, button cell is assembled in glove box, then carries out constant current charge-discharge test.Test result such as Fig. 6 institutes
Show, MXene load Cs eF3Nano-powder is 305.75mAh/g as the discharge capacity first of battery electrode, and MXene is used as electricity
The discharge capacity first of pond electrode is that the lithium battery after 221.0mAh/g, i.e. MXene supported rare earths fluoride nano grain can be substantially
There is higher discharge capacity than pure MXene.Additionally, the nano-powder obtained to embodiment 2 to 5 is also carried out under similarity condition
Constant current charge-discharge test, as a result proves the discharge capacity and two-dimentional carbide Ti of the nano-powder that embodiment 2 to 5 is obtained3C2It is negative
Carry CeF3Nano-powder is suitable, therefore, the nano-powder that embodiment 2 to 5 is obtained also has good application in terms of lithium battery
Prospect.
Finally, it is noted that the foregoing is only the preferred embodiment of the present invention, the present invention is not limited to, it is right
For those skilled in the art, the present invention can have various modifications and variations.It is all within the spirit and principles in the present invention,
Any modification, equivalent substitution and improvements retouching done etc., should be included within the scope of the present invention.
Claims (8)
1. a kind of two-dimentional carbide supported rare earth fluoride nano raw powder's production technology, it is characterised in that comprise the steps：
（1）MAX phase ceramics powder is immersed in the hydrochloric acid solution for being dissolved with lithium fluoride, stir, centrifugation, spend successively from
Sub- water and ethanol purge, gained pressed powder is two-dimentional carbide after being dried；
（2）Two-dimentional carbide is added in rare earth nitrate aqueous solution, 8-24h is placed after stirring evenly, lyophilization obtains two-dimentional carbonization
Thing supported rare earth nitrate composite precursor；Wherein, the concentration of rare earth nitrate aqueous solution is 0.1-1g/mL, per 1mL rare earth nitre
0.5 ~ 1g of two-dimentional carbide is added in acid salt aqueous solution；
（3）Under the protection of argon, 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 body.
2. two-dimentional carbide supported rare earth fluoride nano raw powder's production technology according to claim 1, its feature exists
In step（1）Described in two-dimentional carbide be Ti3C2、Ti2C or V2C。
3. two-dimentional carbide supported rare earth fluoride nano raw powder's production technology according to claim 1, its feature exists
In step（1）Middle rare earth nitrate is Lanthanum (III) nitrate, cerous nitrate, Yttrium trinitrate, Dysprosium trinitrate, Erbium trinitrate, neodymium nitrate, samaric nitrate, nitric acid
At least one in gadolinium and Terbium nitrate (Tb(NO3)3).
4. two-dimentional carbide supported rare earth fluoride nano raw powder's production technology according to claim 3, its feature exists
In step（1）Middle rare earth nitrate is at least one in cerous nitrate and Yttrium trinitrate.
5. two-dimentional carbide supported rare earth fluoride nano raw powder's production technology according to claim 1, its feature exists
In step（1）Middle lyophilization is referred to more than vacuum 20Pa, at least 12h is dried below -20 DEG C of temperature.
6. using two-dimentional carbide supported rare earth fluoride nano powder obtained in the arbitrary described preparation method of claim 1 to 5
Body.
7. application of the two-dimentional carbide supported rare earth fluoride nano powder body described in claim 6 in terms of catalysis hydrogen storage.
8. application of the two-dimentional carbide supported rare earth fluoride nano powder body described in claim 6 in terms of lithium battery.
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| CN109650391A (en) * | 2019-01-29 | 2019-04-19 | 武汉科技大学 | The preparation method of two-dimentional vanadium carbide MXene |
| CN109896524A (en) * | 2019-01-30 | 2019-06-18 | 合肥国轩高科动力能源有限公司 | A kind of preparation method and applications of two dimensional crystal MXene nano material |
| CN110002448A (en) * | 2019-05-10 | 2019-07-12 | 东北大学 | A kind of two dimension rare-earth yttrium carbon compound material and preparation method thereof |
| CN110615440A (en) * | 2019-09-24 | 2019-12-27 | 黑龙江科技大学 | MXene nanosheet with large size and rich oxygen functional group and preparation method and application thereof |
| CN112175275A (en) * | 2020-09-29 | 2021-01-05 | 中北大学 | Mike alkene/ethylene-vinyl acetate copolymer flexible sensing material and preparation method thereof |
| CN113533449A (en) * | 2021-07-05 | 2021-10-22 | 广西师范大学 | Preparation method of MXene graphene composite structure gas sensor |
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| CN113956846A (en) * | 2021-09-28 | 2022-01-21 | 哈尔滨工业大学 | Rare earth oxide nanoparticle doped Mxene material for space charged particle radiation protection, composite coating and preparation method |
| EP4095944A1 (en) * | 2021-05-28 | 2022-11-30 | FDK Corporation | Negative electrode for alkaline storage battery and alkaline storage battery including the negative electrode |
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| CN109650391B (en) * | 2019-01-29 | 2022-03-18 | 武汉科技大学 | Preparation method of two-dimensional vanadium carbide MXene |
| CN109650391A (en) * | 2019-01-29 | 2019-04-19 | 武汉科技大学 | The preparation method of two-dimentional vanadium carbide MXene |
| CN109896524A (en) * | 2019-01-30 | 2019-06-18 | 合肥国轩高科动力能源有限公司 | A kind of preparation method and applications of two dimensional crystal MXene nano material |
| CN110002448A (en) * | 2019-05-10 | 2019-07-12 | 东北大学 | A kind of two dimension rare-earth yttrium carbon compound material and preparation method thereof |
| CN110615440A (en) * | 2019-09-24 | 2019-12-27 | 黑龙江科技大学 | MXene nanosheet with large size and rich oxygen functional group and preparation method and application thereof |
| CN110615440B (en) * | 2019-09-24 | 2022-02-11 | 哈尔滨师范大学 | MXene nanosheet with large size and rich oxygen functional group and preparation method and application thereof |
| CN112175275A (en) * | 2020-09-29 | 2021-01-05 | 中北大学 | Mike alkene/ethylene-vinyl acetate copolymer flexible sensing material and preparation method thereof |
| EP4095944A1 (en) * | 2021-05-28 | 2022-11-30 | FDK Corporation | Negative electrode for alkaline storage battery and alkaline storage battery including the negative electrode |
| CN113533449A (en) * | 2021-07-05 | 2021-10-22 | 广西师范大学 | Preparation method of MXene graphene composite structure gas sensor |
| CN113533449B (en) * | 2021-07-05 | 2023-08-25 | 广西师范大学 | Preparation method of MXene graphene composite structure gas sensor |
| CN113956846A (en) * | 2021-09-28 | 2022-01-21 | 哈尔滨工业大学 | Rare earth oxide nanoparticle doped Mxene material for space charged particle radiation protection, composite coating and preparation method |
| CN113956846B (en) * | 2021-09-28 | 2022-06-17 | 哈尔滨工业大学 | Rare earth oxide nanoparticle doped Mxene material for space charged particle radiation protection, composite coating and preparation method |
| CN113941355A (en) * | 2021-10-18 | 2022-01-18 | 湖北方圆环保科技有限公司 | Preparation method and application of special catalyst for non-methane total hydrocarbon analysis based on MXene |
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