CN110467227A - The high entropy oxide material of novel Ca-Ti ore type and preparation method of the high entropy in five yuan of the position B - Google Patents
The high entropy oxide material of novel Ca-Ti ore type and preparation method of the high entropy in five yuan of the position B Download PDFInfo
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Abstract
The invention discloses a kind of high entropy oxide material of novel Ca-Ti ore type of five yuan of high entropys in the position B and preparation method, the chemical formula of the high entropy oxide material is RE (Cr0.2Fe0.2Mn0.2M0.2N0.2)O3, wherein RE is rare-earth cation La3+、Pr3+、Nd3+、Sm3+、Gd3+And Y3+One of, M and N are bivalent cation Co2+、Ni2+、Mg2+And Zn2+In any two kinds, but do not contain Co simultaneously2+And Ni2+.The present invention, which is realized, has high specific surface area, uniform chemical composition and the high entropy oxide nanocrystalline powder body material of microstructural porous Ca-Ti ore type using solution combustion synthetic method come controllable preparation.The present invention designs the high entropy oxide material with perovskite structure by changing the composition of B cations in perovskite, to customize its physical and chemical performance；Preparation method is easy to operate, practical and convenient for promoting.
Description
Technical field
The present invention relates to high entropy oxide material fields, and in particular to a kind of novel Ca-Ti ore type of the five yuan of high entropys in the position B is high
Entropy oxide material and preparation method.
Background technique
Perofskite type oxide, molecular formula ABO3, wherein A cations are in 12 coordination structures, positioned at cubic cell
12 vertex positions, B cations are in 6 coordination structures, and positioned at the body position of cubic cell, O ion is located at 6 center of area positions
It sets.Since perovskite oxide has composition diversity and unique crystal structure, in thermal stability, chemical stability and structure
There is in terms of stability certain superiority, especially nano-perovskite oxide, be widely used as catalysis material (photocatalysis,
Chemical catalysis and electrochemical catalysis etc.), cathode material for solid-oxide fuel cell, microwave dielectric ceramic material and piezoelectricity pottery
Ceramic material etc..
In recent years, a kind of completely new material for being referred to as high entropy oxide (High-entropy Oxides, HEOs),
Because of its unique performance, such as high thermal stability, unique magnetic performance, efficient lithium ion storge quality, huge Jie
Electrical property and excellent catalytic performance etc. cause the interest of numerous scholars.2015, Rost etc. was for the first time with metal oxide
For raw material, it is successfully prepared using traditional high-temperature solid phase reaction method with single rock-salt type structure
(Co0.2Cu0.2Mg0.2Ni0.2Zn0.2) O HEO block materials (C.M.Rost, E.Sachet, T.Borman, A.Moballegh,
E.C.Dickey,D.Hou,J.L.Jones,S.Curtarolo,J.P.Maria,Entropy-stabilized oxides,
Nat.Commun.,6(2015)8485-8491.).Hereafter, a series of other types of high entropy oxides, as fluorite type, point are brilliant
The solid solution structures such as stone-type and Ca-Ti ore type are prepared out in succession.
Sarkar in 2018 etc. is designed and spray pyrolysis is used to be prepared for 12 kinds A as rare-earth cation (Rare
Earth, RE, Gd3+、La3+、Nd3+、Sm3+And Y3+), B are transition-metal cation (Transition Metal, TM, Co2+、
Cr3+、Fe3+、Mn2+And Ni2+) oxide powder material, research finds.The single Ca-Ti ore type knot of only 6 kinds of System formings
(the Gd of structure, respectively A high entropy0.2La0.2Nd0.2Sm0.2Y0.2)CoO3, B high entropys Gd (Co0.2Cr0.2Fe0.2Mn0.2Ni0.2)
O3、La(Co0.2Cr0.2Fe0.2Mn0.2Ni0.2)O3With Nd (Co0.2Cr0.2Fe0.2Mn0.2Ni0.2)O3And A, B are high entropy
(Gd0.2La0.2Nd0.2Sm0.2Y0.2)(Co0.2Cr0.2Fe0.2Mn0.2Ni0.2)O3High entropy oxide powder material (A.Sarkar,
R.Djenadic,D.Wang,C.Hein,R.Kautenburger,O.Clemens,H.Hahn,Rare earth and
transition metal based entropy stabilised perovskite type oxides,
J.Eur.Ceram.Soc.,38(2018)2318-2327.).Hereafter Jiang etc. is prepared for using mechanical ball mill+solid sintering technology
Ba(Zr0.2Sn0.2Ti0.2Hf0.2Nb0.2)O3Etc. a series of high entropy oxide block materials of Ca-Ti ore type of B high entropys
(S.Jiang,T.Hu,J.Gild,N.Zhou,J.Nie,M.Qin,T.Harrington,K.Vecchio,J.Luo,A new
class of high-entropy perovskite oxides,Scripta Mater.,142(2018)116-120.)。
Sharma etc. is prepared for Ba (Zr using pulsed laser deposition0.2Sn0.2Ti0.2Hf0.2Nb0.2)O3The high entropy oxide of Ca-Ti ore type
Thin-film material (Y.Sharma, B.L.Musico, X.Gao, C.Hua, A.F.May, A.Herklotz, A.Rastogi,
D.Mandrus,J.Yan,H.N.Lee,M.F.Chisholm,V.Keppens,T.Z.Ward,Single-crystal high
entropy perovskite oxide epitaxial films,Phys.Rev.Mater.,2(2018)060404-
060406.).Chinese patent CN 109650876 and CN109607615 is prepared for A high entropys using solid sintering technology respectively
(La0.2Li0.2Ba0.2Sr0.2Ca0.2)TiO3With the Ba (Zr of B high entropys1/6Sn1/6Ti1/6Hf1/6Nb1/6)O3The high entropy oxygen of Ca-Ti ore type
Compound material.
At present about the research of the high entropy oxide of Ca-Ti ore type also in the initial stage, existing research is only limitted to above-mentioned several
Kind, further to expand the high entropy oxide of Ca-Ti ore type, meets some special use demands, can be designed a kind of five yuan of position B
The high entropy oxide material of the novel Ca-Ti ore type of high entropy.The high entropy oxide of the series perovskite type is not yet retrieved at present, especially
It is the relevant report of Ca-Ti ore type nanocrystalline powder.
Summary of the invention
There is provided a kind of high entropy oxide materials of novel Ca-Ti ore type of five yuan of high entropys in the position B for the first aspect of the invention
Material；Another aspect of the present invention is also resided in using a kind of easy to operate, practical and convenient for popularization preparation method-solution
Combustion method obtains the nanocrystalline high entropy oxide powder material of high-specific surface area and porous structure.
In order to achieve the above object, the present invention is achieved by the following technical programs:
A kind of high entropy oxide material of novel Ca-Ti ore type of the five yuan of high entropys in the position B, the chemistry of the high entropy oxide material
Formula is RE (Cr0.2Fe0.2Mn0.2M0.2N0.2)O3, wherein RE is rare-earth cation La3+、Pr3+、Nd3+、Sm3+、Gd3+And Y3+In
It is a kind of；M, N is bivalent cation Co2+、Ni2+、Mg2+And Zn2+In any two kinds, but not simultaneously be Co2+And Ni2+。
The preparation method of the high entropy oxide material of novel Ca-Ti ore type of above-mentioned five yuan of high entropys in the position B, which is characterized in that including
Following steps:
(1) by various rare earth nitrades and metal nitrate according to molecular formula RE (Cr0.2Fe0.2Mn0.2M0.2N0.2)O3Change
Metering is learned than carrying out precise, is dissolved in a certain amount of distilled water, is stirred at room temperature uniformly, obtain containing a kind of rare earth sun
The mixed solution of ion and five kinds of metal cations；
(2) a certain amount of fuel is weighed, above-mentioned mixed solution is added, is stirred at room temperature uniformly, obtains transparent colloidal sol；
(3) above-mentioned transparent colloidal sol is placed in 80~150 DEG C of baking ovens, evaporates moisture therein, obtain gel；
(4) this gel is placed in high-temperature service, heat preservation a period of time obtains B as five yuan of height at 750~1000 DEG C
The high entropy oxide material nanocrystalline powder material of the Ca-Ti ore type of entropy.
Preferably, in step (1), the concentration of rare-earth cation is 1.0mol/L~2.0mol/L in the mixed solution.
Preferably, in step (1), the concentration of metal cation is 0.2mol/L~0.4mol/L in the mixed solution.
Preferably, in step (2), the fuel is glycine, tartaric acid, citric acid, Beta-alanine, six methylene four
The mixing of one or more of amine and polyethylene glycol (PEG), but it is not limited to above-mentioned fuel.
Preferably, in step (2), the molar ratio of the fuel and metal cation is 0.2~2:1.
Preferably, in step (4), the high-temperature service is Muffle furnace or gold furnace.
Preferably, in step (4), 0.5~1h is kept the temperature at 750~1000 DEG C.
The beneficial effects of the present invention are:
The present invention designs the high entropy oxide with perovskite structure by changing the composition of B cations in perovskite
Material meets some special use demands to customize its physical and chemical performance；In addition, using solution combustion method preparation
The porous high entropy oxide nanocrystalline powder specific surface area with higher of Ca-Ti ore type, uniform chemical composition and microstructure,
It is convenient for the regulation of microstructure, it is final to realize that performance regulates and controls on demand.Preparation method is easy to operate, practical and convenient for pushing away
Extensively.
Detailed description of the invention
Fig. 1 is embodiment 1La (Cr0.2Fe0.2Mn0.2Ni0.2Zn0.2)O3The XRD diagram piece of high entropy oxide powder；
Fig. 2 is embodiment 1La (Cr0.2Fe0.2Mn0.2Ni0.2Zn0.2)O3The SEM picture of high entropy oxide powder；
Fig. 3 is embodiment 2Y (Cr0.2Fe0.2Mn0.2Mg0.2Ni0.2)O3The SEM picture of high entropy oxide powder；
Fig. 4 is embodiment 3Pr (Cr0.2Fe0.2Mn0.2Co0.2Zn0.2)O3The SEM picture of high entropy oxide powder.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is the present invention one
Divide embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making
Every other embodiment obtained, shall fall within the protection scope of the present invention under the premise of creative work.
Embodiment 1:
The high entropy oxide powder of novel Ca-Ti ore type of the high entropy in five yuan of the position B, high entropy oxide are prepared using solution combustion method
The chemical composition of powder is La (Cr0.2Fe0.2Mn0.2Ni0.2Zn0.2)O3: it is weighed according to the stoichiometric ratio of molecular formula corresponding dilute
Native nitrate and metal nitrate, the La (NO of specially 4.330g3)3.9H2O, the Cr (NO of 0.8004g3)3.9H2O、0.808g
Fe (NO3)3.9H2O, the Mn (NO of 0.574g3)2.4H2O, the Ni (NO of 0.582g3)2.6H2Zn (the NO of O and 0.595g3)2.6H2O is dissolved in 10mL distilled water, is stirred at room temperature uniformly, obtain containing a kind of rare-earth cation and five kinds of metal sun from
The mixed solution of son；Then it weighs 6.006g glycine to be added in above-mentioned mixed solution, stir evenly；It then will be above-mentioned transparent molten
Glue is placed in 100 DEG C of baking oven be dried and evaporated moisture after obtain sticky gel；Finally above-mentioned gel is placed in Muffle furnace,
And in 1000 DEG C of heat preservation 1h, obtaining crystal structure is Ca-Ti ore type, specific surface area 18m2/ g, average grain size are 48nm's
Porous La (Cr0.2Fe0.2Mn0.2Ni0.2Zn0.2)O3Powder body material, XRD diagram piece, SEM the picture institute as shown in Figure 1, Figure 2 of the powder body material
Show.
Embodiment 2:
The high entropy oxide powder of novel Ca-Ti ore type of the high entropy in five yuan of the position B, high entropy oxide are prepared using solution combustion method
The chemical composition of powder is Y (Cr0.2Fe0.2Mn0.2Mg0.2Ni0.2)O3: it is weighed according to the stoichiometric ratio of molecular formula corresponding dilute
Native nitrate and metal nitrate, the Y (NO of specially 2.794g3)3.nH2O, the Cr (NO of 0.8004g3)3.9H2O, 0.808g
Fe(NO3)3.9H2O, the Mn (NO of 0.574g3)2.4H2O、0.513gMg(NO3)2.6H2Ni (the NO of O and 0.582g3)2.6H2O, it is molten
In 10mL distilled water, it is stirred at room temperature uniformly, obtains the mixing containing a kind of rare-earth cation and six kinds of metal cations
Solution；Then it weighs 6.004g tartaric acid to be added in above-mentioned mixed solution, stir evenly；Then above-mentioned vitreosol is placed in
Sticky gel is obtained after being dried and evaporated moisture in 100 DEG C of baking oven；Above-mentioned gel is finally placed in gold furnace, and at 800 DEG C
2h is kept the temperature, obtaining specific surface area is 32m2/ g, the porous Y of Ca-Ti ore type that average grain size is 30nm
(Cr0.2Fe0.2Mn0.2Mg0.2Ni0.2)O3The SEM picture of powder body material, the powder body material is as shown in Figure 3.
Embodiment 3:
The high entropy oxide powder of novel Ca-Ti ore type of the high entropy in five yuan of the position B, high entropy oxide are prepared using solution combustion method
The chemical composition of powder is Pr (Cr0.2Fe0.2Mn0.2Co0.2Zn0.2)O3: it is weighed according to the stoichiometric ratio of molecular formula corresponding dilute
Native nitrate and metal nitrate, the Pr (NO of specially 3.269g3)3.9H2O, the Cr (NO of 0.8004g3)3.9H2O、0.808g
Fe (NO3)3.9H2O, the Mn (NO of 0.574g3)2.4H2O, the Co (NO of 0.582g3)2.6H2Zn (the NO of O and 0.595g3)2.6H2O is dissolved in 8mL distilled water, is stirred at room temperature uniformly, is obtained containing a kind of rare-earth cation and six kinds of metal cations
Mixed solution；Then it weighs 1.921g citric acid to be added in above-mentioned mixed solution, stir evenly；Then by above-mentioned vitreosol
It is placed in 150 DEG C of baking oven after being dried and evaporated moisture and obtains sticky gel；Finally above-mentioned gel is placed in Muffle furnace, and
In 750 DEG C of heat preservation 30min, obtaining specific surface area is 48m2/ g, the porous Pr of Ca-Ti ore type that average grain size is 16nm
(Cr0.2Fe0.2Mn0.2Co0.2Zn0.2)O3The SEM picture of powder body material, the powder body material is as shown in Figure 4.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
Invention is explained in detail, those skilled in the art should understand that: it still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features；And these modification or
Replacement, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (8)
- The high entropy oxide material of novel Ca-Ti ore type of the high entropy in five yuan of the position 1.B, which is characterized in that the high entropy oxide material Chemical formula is RE (Cr0.2Fe0.2Mn0.2M0.2N0.2)O3, wherein RE is rare-earth cation La3+、Pr3+、Nd3+、Sm3+、Gd3+And Y3+ One of；M, N is bivalent cation Co2+、Ni2+、Mg2+And Zn2+In any two kinds, but not simultaneously be Co2+And Ni2+。
- 2. a kind of preparation method of the high entropy oxide material of novel Ca-Ti ore type of five yuan of high entropys in the position B as described in claim 1, It is characterized by comprising the following steps:(1) by various rare earth nitrades and metal nitrate according to molecular formula RE (Cr0.2Fe0.2Mn0.2M0.2N0.2)O3Chemistry meter Amount is dissolved in a certain amount of distilled water than carrying out precise, is stirred at room temperature uniformly, obtains containing a kind of rare-earth cation With the mixed solution of five kinds of metal cations；(2) a certain amount of fuel is weighed, above-mentioned mixed solution is added, is stirred at room temperature uniformly, obtains transparent colloidal sol；(3) above-mentioned transparent colloidal sol is placed in 80~150 DEG C of baking ovens, evaporates moisture therein, obtain gel；(4) this gel is placed in high-temperature service, it is five yuan of high entropys that heat preservation a period of time, which obtains B, at 750~1000 DEG C The high entropy oxide material nanocrystalline powder material of Ca-Ti ore type.
- 3. a kind of preparation method of the high entropy oxide material of novel Ca-Ti ore type of the five yuan of high entropys in the position B as claimed in claim 2, It is characterized in that, the concentration of rare-earth cation is 1.0mol/L~2.0mol/L in the mixed solution in step (1).
- 4. a kind of preparation method of the high entropy oxide material of novel Ca-Ti ore type of the five yuan of high entropys in the position B as claimed in claim 2, It is characterized by: the concentration of metal cation is 0.2mol/L~0.4mol/L in the mixed solution.
- 5. a kind of preparation method of the high entropy oxide material of novel Ca-Ti ore type of the five yuan of high entropys in the position B as claimed in claim 2, It is characterized in that, in step (2), the fuel be glycine, tartaric acid, citric acid, Beta-alanine, hexamethylene tetramine and The mixing of one or more of polyethylene glycol.
- 6. a kind of preparation method of the high entropy oxide material of novel Ca-Ti ore type of the five yuan of high entropys in the position B as claimed in claim 2, It is characterized in that, the molar ratio of the fuel and metal cation is 0.2~2:1 in step (2).
- 7. a kind of preparation method of the high entropy oxide material of novel Ca-Ti ore type of the five yuan of high entropys in the position B as claimed in claim 2, It is characterized in that, the high-temperature service is Muffle furnace or gold furnace in step (4).
- 8. a kind of preparation method of the high entropy oxide material of novel Ca-Ti ore type of the five yuan of high entropys in the position B as claimed in claim 2, It is characterized in that, keeping the temperature 0.5~1h at 750~1000 DEG C in step (4).
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