CN108821351A - A kind of preparation method of the porous high entropy oxide material of spinel-type - Google Patents
A kind of preparation method of the porous high entropy oxide material of spinel-type Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of the porous high entropy oxide material of spinel-type, belong to inorganic oxide powder Material Field.This method is low-temperature combustion synthesis, specifically:Use metal nitrate for source metal, the mixture of one or more of citric acid, ethylenediamine tetra-acetic acid, hexamethylene tetramine and glucose is fuel, regulates and controls the high entropy oxide (CoCrFeMnNi) of spinel-type transition metal by controlling concentration, the type of fuel and additional amount, the type of combustion adjuvant and additional amount and the sparking mode of metal salt raw material3O4The characteristics such as the granularity of nano-powder and pattern.This preparation method uses liquid phase ingredient, it is ensured that raw material reaches molecular level mixing, and product realizes stoichiometric ratio;Simultaneously energy saving, high production efficiency, it is environmentally protective, without complicated post-processing the advantages that.High entropy oxide powder purity is high, even particle size distribution prepared by the present invention.
Description
Technical field
The invention belongs to inorganic oxide powder Material Field, in particular to a kind of high entropy oxygen of lithium ion battery negative material
The preparation method of compound material specially has spinel-type porous (CoCrFeMnNi)3O4The preparation side of high entropy oxide material
Method.
Background technique
Lithium ion battery is moved because it has many advantages, such as that light-weight, small in size, energy density is high, cycle performance is good
The extensive pro-gaze in the fields such as the portable electronic products such as mobile phone, laptop and new-energy automobile.Lithium ion battery is negative
Pole material plays important function in terms of the capacity and cycle performance for improving battery, and performance directly affects lithium ion battery
Performance.Commercial lithium ion battery negative material is generally graphite-like carbon negative pole material at present, but its theoretical specific capacity is only
For 372mAhg-1And it is unfavorable for battery and relevant apparatus and develops to miniaturization, while the intercalation potential of graphite-based cathode is close
The current potential of lithium metal is unfavorable for the safety of battery.It is above-mentioned that there are problems strictly to limit the development of the following lithium ion battery.Therefore
Developing, there is the lithium ion battery negative material of higher capacity to be particularly important.
In recent years, transition metal oxide had received extensive concern as lithium ion battery negative material.It is Chinese special
Application No. is 201410276284.7 to disclose a kind of transition metal oxide M for benefitxOy(M Fe, one of Mn and Cr or several
Kind) lithium ion battery negative material.Binary lithium ion battery negative material is developed on this basis, if Liu Lei is with hydro-thermal
Synthetic method is prepared for NiFe2O4、ZnFe2O4、CoxFe3-xO4、CoxMn3-xO4And wait two with spinel structure of binary series
Powder negative electrode material (the knot of Liu Lei lithium ion battery transition metal oxide negative electrode material of first oxide as lithium ion battery
Structure design and Electrochemical Properties Chinese Academy of Sciences University Ph.D. Dissertation, 2015.).Chinese Patent Application No. is at present
201711421445.7 proposing to be prepared for using the laser molecular beam epitaxy precipitation method for lithium ion battery negative material
(MgCoNiCuZn) O high entropy oxide film material.
High entropy oxide material is a kind of new ceramic material to grow up on the basis of high-entropy alloy, beauty in 2015
The Christina M.Rost of state is put forward for the first time on the basis of high-entropy alloy.2018Deng being prepared for having for the first time
There is (CoCrFeMnNi) of spinel structure2O3High entropy oxide block materials, this method is by five kinds of oxides of equimolar ratio
NiO、MnO、Co3O4、Fe2O3And Cr2O3In vibrating mill mixing 25min;Then uniformly mixed raw material are pressed into 9 ×
The cylindrical body of 1.5mm;Followed by hot isostatic pressing technique, 20h is calcined at 200MPa, 1050 DEG C;Finally utilize cooling aluminium
Corresponding high entropy oxide block materials (J. is made in rapid cooling to plate in airM.Stygar, A.
A.Knapik, K.Mroczka, W.Tejchman, M.Danielewski, M.Martin, Synthesis and
microstructure of the(CoCrFeMnNi)3O4high entropy oxide characterized by spinel
Structure, Materials Letters, 216 (2018) 32-36.).The method use vibrating mill mixing, although the time compared with
It is short, can be to avoid the introducing of impurity, but be inevitable there are the non-uniform phenomenon of raw material mixing, so that use heat
The block materials of isostatic pressing method preparation have the defects that institutional framework is inhomogenous.Therefore there is the high entropy oxidate powder of single solid solution phase
The successful preparation of body material is the prerequisite for obtaining institutional framework uniform block body ceramic material and coating material.Germany
A.Sarkar etc. is prepared for nanocrystalline multicomponent entropy stabilization transition metal oxide (CoCuMgNiZn) O powder using pyrolysis spray-on process
Body material (A.Sarkar, R.Djenadic, N.J.Usharani, K.P.Sanghvi, V.S.K.Chakravadhanula,
A.S.Gandhi, H.Hahn, S.S.Bhattacharya, Nanocrystalline multicomponent entropy
Stabilised transition metal oxides, Journal of the European Ceramic Society, 37
(2017) 747-754.), which equally exists the disadvantages of preparation process is complicated, and energy consumption is high.
In recent years, SHS process (Self-propagating High-temperature Synthesis, letter
It is written as SHS) low-temperature combustion synthesis (Low-temperature Combustion has been developed in conjunction with wet chemistry method
Synthesis is abbreviated as LCS).On the one hand the method uses liquid phase ingredient, it is ensured that raw material reaches molecular level mixing, and product is realized
Stoichiometric ratio;On the other hand after lower temperature (200-500 DEG C) ignites, using own combustion heat release make to react it is spontaneous into
Row, conbustion synthesis speed is fast, so that the product of preparation has the characteristics that dispersion degree is high, chemical uniformity is good and partial size is thin.At present
Not yet retrieve that prepare spinel-type using low-temperature burning porous (CoCrFeMnNi)3O4The correlation of high entropy oxide powder material
Report.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the prior art, such as mechanical alloying method and pyrolysis spray-on process preparation
High entropy oxide powder material the deficiencies in the prior art, provide a kind of energy saving, high production efficiency, it is environmentally protective, without multiple
It is porous (CoCrFeMnNi) that miscellaneous post-processing can be prepared by the spinel-type that with high purity, granularity is tiny and is evenly distributed3O4High entropy oxygen
The preparation method of compound powder body material.
Spinel-type provided by the invention is porous (CoCrFeMnNi)3O4The preparation method of high entropy oxide material is specific to wrap
Include following steps:
(1) nitrate for weighing Co, Cr, Fe, Mn and Ni of equimolar amounts, is dissolved in a certain amount of distilled water or ethyl alcohol is water-soluble
It in liquid, stirs evenly, obtains the mixed solution containing metal salt.Wherein in ethanol water volume fraction of ethanol be 15~
85%.The concentration of the metal salt is 1~2mol/L.
(2) mixture of a certain amount of fuel or fuel and combustion adjuvant is weighed in above-mentioned mixed solution, is stirred evenly simultaneously
The pH that appropriate ammonium hydroxide adjusts mixed solution is added, obtains transparent colloidal sol;Wherein:The pH range of the solution is adjusted to 6~8,
The molar ratio of the fuel and nitrate metal ion is 1~3: 1.In the mixture of the fuel and combustion adjuvant:Combustion adjuvant institute
Accounting for mass ratio is 1.5~3%.
(3) mixing for above-mentioned vitreosol being placed in water or second alcohol and water in heating evaporation colloidal sol in water-bath or oil bath is molten
Agent obtains loose, foam-like gel, and temperature when evaporating solvent is 80~200 DEG C.
(4) this gel is placed in 300~500 DEG C of Muffle furnace, or is placed directly in micro-wave oven, low-temperature burning reaction occurs
Obtain required nanoscale, porous (CoCrFeMnNi) with rock-salt type structure3O4High entropy oxide powder material.Wherein exist
The reaction time is 15~30min in Muffle furnace;Microwave input power is 600~700W, and the reaction time is 4~10min.
The fuel is one or more of citric acid, ethylenediamine tetra-acetic acid, hexamethylene tetramine and glucose
Mixing.
The combustion adjuvant is one or both of ammonium acetate and ammonium nitrate.
The spinel-type that above-mentioned preparation method obtains is porous (CoCrFeMnNi)3O4High entropy oxide material can lithium from
It is applied in sub- cell negative electrode material.
Compared with prior art, the beneficial effects of the invention are as follows:
(1) liquid phase ingredient is used, it is ensured that raw material reaches molecular level mixing, and product realizes stoichiometric ratio;
(2) low-temperature combustion synthesis is used, is ignited in lower temperature, main reaction moment completes, and low energy consumption, production cost
It is low;
(3) reaction process is environmentally protective, and product is without complicated last handling process;
(4) it production die tiny (40nm~130nm) and is evenly distributed.
Detailed description of the invention
Fig. 1 is made from embodiment 1 (CoCrFeMnNi)3O4The XRD diagram piece of high entropy oxide powder.
Fig. 2 is made from embodiment 1 (CoCrFeMnNi)3O4The SEM picture of high entropy oxide powder.
Fig. 3 is made from embodiment 2 (CoCrFeMnNi)3O4The SEM picture of high entropy oxide powder.
Specific embodiment
The present invention is described in detail below in conjunction with specific embodiment, but the present invention is not limited to following embodiments.
Embodiment 1
Weigh the Co (NO of 14.55g3)2·6H2O, the Cr (NO of 20.008g3)3·9H2O, the Fe (NO of 20.2g3)3·
9H2O, the Mn (NO of 12.55g3)2·4H2Ni (the NO of O and 14.54g3)2·6H2O is dissolved in 50mL distilled water, is stirred evenly
To the mixed solution containing metal salt;Then it weighs 48.03g citric acid and 0.72g ammonium nitrate is added in above-mentioned mixed solution, stir
Adjusting the pH of mixed solution after mixing uniformly with ammonium hydroxide is 8, obtains transparent colloidal sol;Then above-mentioned vitreosol is placed in 150 DEG C
Oil bath in heating to remove aqueous solvent, obtain loose, foam-like gel;Above-mentioned gel is finally placed in 300 DEG C of Muffle
Furnace reacts 30min, obtains final products.XRD spectra (Fig. 1) shows prepared (CoCrFeMnNi)3O4High entropy oxide material
For spinel structure, SEM picture (Fig. 2) shows prepared (CoCrFeMnNi)3O4The average grain diameter of high entropy oxide material is
40nm, pattern are spherical and have porous structure.
Embodiment 2
Weigh the Co (NO of 29.01g3)2·6H2O, the Cr (NO of 40.02g3)3·9H2O, the Fe (NO of 40.4g3)3·9H2O、
Mn (the NO of 25.10g3)2·4H2Ni (the NO of O and 29.08g3)2·6H2O be dissolved in 42.5mL distilled water and 7.5mL ethyl alcohol composition
In solvent, it is uniformly mixing to obtain the mixed solution containing metal salt;Then 162.14g glucose and 29.22g ethylenediamine tetraacetic are weighed
Acetic acid is added in above-mentioned mixed solution, is after mixing evenly 6 with the pH that ammonium hydroxide adjusts mixed solution, obtains transparent colloidal sol;It connects
Above-mentioned vitreosol is placed in 120 DEG C of oil bath and heats to remove aqueous solvent, obtain loose, foam-like gel;Finally
Above-mentioned gel is placed in the micro-wave oven that input power is 700W and reacts 10min, obtains final products.SEM picture (Fig. 3) shows
Prepared (CoCrFeMnNi)3O4The average grain diameter of high entropy oxide material is 90nm, and pattern is spherical and has porous knot
Structure.
Embodiment 3
Weigh the Co (NO of 21.83g3)2·6H2O, the Cr (NO of 30.01g3)3·9H2O, the Fe (NO of 30.3g3)3·9H2O、
Mn (the NO of 18.83g3)2·4H2Ni (the NO of O and 21.81g3)2·6H2O is dissolved in 42.5mL ethyl alcohol and 7.5mL distilled water, is stirred
It mixes and uniformly obtains the mixed solution containing metal salt;Then it weighs 101.34g glucose and above-mentioned mixing is added in 3.04g ammonium acetate
In solution, it is after mixing evenly 7 with the pH that ammonium hydroxide adjusts mixed solution, obtains transparent colloidal sol;Then by above-mentioned vitreosol
It is placed in 80 DEG C of water-bath and heats to remove aqueous solvent, obtain loose, foam-like gel;Above-mentioned gel is finally placed in 500
DEG C Muffle furnace react 10min, obtain average grain diameter be 130nm spherical spinel type (CoCrFeMnNi)3O4High entropy oxide
Powder body material.
Claims (5)
1. a kind of preparation method of the porous high entropy oxide material of spinel-type, it is characterised in that include the following steps:
(1) nitrate for weighing Co, Cr, Fe, Mn and Ni of equimolar amounts is dissolved in distilled water or ethanol water, and stirring is equal
It is even, obtain the mixed solution containing metal salt;
Volume fraction of ethanol is 15~85% in the ethanol water;The concentration of the metal salt is 1~2mol/L;
(2) mixed solution that step (1) obtains is added in the mixture for weighing fuel or fuel and combustion adjuvant, stirs evenly and adds
Enter the pH to 6~8 that ammonium hydroxide adjusts mixed solution, obtains transparent colloidal sol;
The molar ratio of the metal ion of the fuel and mixed solution is 1~3: 1;In the mixture of the fuel and combustion adjuvant:
Mass ratio shared by combustion adjuvant is 1.5%~3%;
(3) above-mentioned vitreosol is placed in water-bath or oil bath the mixed solvent of water or second alcohol and water in heating evaporation colloidal sol, obtained
Obtain loose, foam-like gel;
(4) gel that step (3) obtains is placed in 300~500 DEG C of Muffle furnace, or be placed directly in micro-wave oven, low temperature occurs
Target product is obtained after combustion reaction;
Wherein:The reaction time is 15~30min in Muffle furnace;Microwave input power be 600~700W, the reaction time be 4~
10min。
2. the preparation method of the porous high entropy oxide material of spinel-type according to claim 1, which is characterized in that described
Fuel is one or more of citric acid, ethylenediamine tetra-acetic acid, hexamethylene tetramine and glucose.
3. the preparation method of the porous high entropy oxide material of spinel-type according to claim 1, which is characterized in that described
Combustion adjuvant is one or both of ammonium acetate and ammonium nitrate.
4. the preparation method of the porous high entropy oxide material of spinel-type according to claim 1, which is characterized in that described
The temperature that step (3) evaporates solvent is 80~200 DEG C.
5. the porous high entropy oxide material of the spinel-type that preparation method obtains according to claim 1 is negative in lithium ion battery
Application in the material of pole.
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CN110104648A (en) * | 2019-05-10 | 2019-08-09 | 东华大学 | A kind of high entropy carbide nano powder and preparation method thereof |
CN110364717A (en) * | 2019-07-24 | 2019-10-22 | 东北大学秦皇岛分校 | A kind of high entropy oxide electrode material of spinel-type and preparation method thereof |
CN110526706A (en) * | 2019-09-19 | 2019-12-03 | 安徽工业大学 | A kind of high entropy oxide powder material of eutectic and preparation method |
CN110556536A (en) * | 2019-09-19 | 2019-12-10 | 安徽工业大学 | Six-element high-entropy oxide material for lithium ion battery and preparation method thereof |
CN110563462A (en) * | 2019-09-19 | 2019-12-13 | 安徽工业大学 | B-site six-element high-entropy novel perovskite type high-entropy oxide material and preparation method thereof |
CN110600703A (en) * | 2019-09-19 | 2019-12-20 | 安徽工业大学 | Five-element transition metal oxide high-entropy material for lithium ion battery |
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CN111348910A (en) * | 2020-03-10 | 2020-06-30 | 南昌航空大学 | Hexahydric spinel type iron-cobalt-chromium-manganese-nickel-copper series high-entropy oxide and powder preparation method thereof |
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CN110600703A (en) * | 2019-09-19 | 2019-12-20 | 安徽工业大学 | Five-element transition metal oxide high-entropy material for lithium ion battery |
CN110600703B (en) * | 2019-09-19 | 2022-09-30 | 安徽工业大学 | Five-element transition metal oxide high-entropy material for lithium ion battery |
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