CN107381649A - A kind of europium cation doping ferrite composite material and preparation method thereof - Google Patents
A kind of europium cation doping ferrite composite material and preparation method thereof Download PDFInfo
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- CN107381649A CN107381649A CN201710433817.1A CN201710433817A CN107381649A CN 107381649 A CN107381649 A CN 107381649A CN 201710433817 A CN201710433817 A CN 201710433817A CN 107381649 A CN107381649 A CN 107381649A
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Abstract
The invention discloses a kind of europium cation doping ferrite composite material, cabaltous nitrate hexahydrate, six nitric hydrate europiums and Fe(NO3)39H2O are dissolved in deionized water by the amount ratio of different materials, pH is adjusted to alkalescence by NaOH, using easy one step hydro thermal method, rod-like nano europium is made and has mixed cobalt ferrite material.This method technological process is simple, simple to operate easy to control.
Description
Technical field
The present invention relates to technical field of composite materials, more particularly to a kind of europium cation doping ferrite composite material and its preparation
Method.
Background technology
Spinel-type Conjugate ferrite belongs to a kind of ferrimagnetic material, and it has unique physics, chemical property and magnetic
Matter.Its higher high frequency magnetic conductivity, magnetocrystalline heteromerism, and tens times higher than magnetic alloy of coercivity and resistivity, make
Be widely used in communication broadcast, mutual inductance device, magnetic core bearing, microwave absorption etc..For existing Conjugate ferrite
Production technology, easy to operate easily controllable, thin slice is rolled into unlike metallicl magnetic material or fine powder medium is made to answer
With.In recent years, magnetic Nano material gets more and more people's extensive concerning, and developing different types of Nanometer Cobalt Ferrite Oxide also turns into mesh
The hot issue of preceding magnetic material research.
Single Conjugate ferrite is not wide enough in the suction wave frequency band of low-frequency range, and density is big, and with the rise of temperature, it absorbs ripple
It is able to can weaken.There are some researches show, rare earth element because it is due to its special space structure, can be doped with Conjugate ferrite,
So as to improve the electromagnetic performance of Conjugate ferrite.At present on Eu2+Adulterate the influence for Conjugate ferrite structure and magnetic and its shadow
The mechanism of sound is rarely reported, and different preparation methods can prepare the Conjugate ferrite of different appearances, and its purpose is provided to
To more preferable electromagnetic performance.
The content of the invention
Based on technical problem existing for background technology, the present invention proposes a kind of europium cation doping ferrite composite material, should
Composite is club shaped structure, possesses good electromagnetic performance.
A kind of europium cation doping ferrite composite material, chemical formula CoxEu1-xFe2O4, wherein x=0.80,0.85,0.90,
0.95, its structure is club shaped structure.
A kind of preparation method of europium cation doping ferrite composite material, method and step are as follows：
S1：Europium nitrate, cobalt nitrate and ferric nitrate are sequentially added in deionized water, is stirred；Then it is added dropwise
NaOH solution, the pH of solution is adjusted to alkalescence and continues to stir；
S2:Solution obtained by S1 is moved into isothermal reaction in reactor.After the completion of reaction, solution is cooled to room temperature, used
It is multiple that deionized water and ethanol will precipitate washing repeatedly；
S3:Finally dry the product in vacuum drying chamber.
Preferably, the metal salt sequentially added in the S1 is six nitric hydrate europiums, cabaltous nitrate hexahydrate, nine nitric hydrates
Iron.
Preferably, the six nitric hydrates europium, cabaltous nitrate hexahydrate, the amount of material of Fe(NO3)39H2O are 0.1-0.4:
1.6-1.9:4。
Preferably, the concentration of NaOH solution is 3-5mol/L in the S1, and the pH value of solution is 10-12.
Preferably, the reaction temperature of isothermal reaction kettle is 160-180 DEG C in the S2, reaction time 10-12h.
Preferably, vacuum drying condition is that 12h is dried at 60 DEG C in the S3.
A kind of europium cation doping ferrite composite material proposed by the present invention is prepared as stated above.
Compared with the prior art, the present invention has the beneficial effect that：
1st, the bar-shaped spinel-type cobalt europium ferrite of two dimension can be prepared by the technology of the present invention.Cobalt ions and iron ion are because heavy
The addition of shallow lake agent sodium hydroxide forms iron hydroxide and cobalt hydroxide presoma, then forms Conjugate ferrite nucleus by hydro-thermal,
The europium ion being subsequently added into forms specific growth because its larger radius destroys the original orientation of growth of Conjugate ferrite crystal
Orientation.It can be learnt from XRD, for the diffraction maximum at 2 θ=35.62 ° relative to other appearances, peak intensity is higher and sharp, represents
The crystal growth degree of orientation is high, is more likely formed club shaped structure.
2nd, this two-dimensional nanostructure of nano bar-shape material is easy to carrier free movement, i.e., electric conductivity compare with it is of the same race
Other patterns of material are outstanding.Club shaped structure has larger surface area compared to other patterns, causes unsaturated bond and dangling bonds to increase
It is more, improve the surface-active of material, be easy in other materials of bar-shaped surface modification, and if nano-bar material along magnetization direction of principal axis
Growth, will be greatly improved magnetization property.
3rd, in the present invention, by Eu2+It is doped into Conjugate ferrite, Eu2+Strong Quantum geometrical phase angular momentum can be to ferro-cobalt
The magnetic anisotropy of oxysome produces contribution, improves the coercivity of Conjugate ferrite.Meanwhile work as Eu2+After entering Conjugate ferrite, because
Its electronic shell is unfilled, can produce unmatched magnetic moment, and booster action is played to magnesium-yttrium-transition metal atomic magnetic moment, improves ferro-cobalt
The saturation magnetization of oxysome.
4th, rare earth element is due to its special space structure, if absorbing material can be improved by being entrained in absorbing material
Peak value, broadening absorption band.The europium element used in the present invention, minimum in rare earth element Midst density, material is most soft, and it is entrained in
The density and hardness of Conjugate ferrite can be effectively reduced in Conjugate ferrite, it is more agreed with novel wave-absorbing material easily moulding and material
Light two major features.
5th, the cobalt europium ferrite that the present invention is prepared using hydro-thermal method, any surfactant, less pollution, green are not added
Environmental protection.Preparation method is simple, and the cobalt europium ferrite of preparation does not need subsequent treatment, high-temperature calcination under such as protective gas atmosphere.Energy
Source consumption is few, is easy to the advantages such as industrialization；React easy to control, it is not necessary to expensive equipment, process stabilizing, be easy to repeat.
Brief description of the drawings
Fig. 1 is the ferritic X-ray diffractogram of europium cation doping made from embodiment 1；
Fig. 2 is the ferritic TEM figures of europium cation doping made from embodiment 1；
Fig. 3 is the ferritic TEM figures of europium cation doping made from embodiment 2；
Fig. 4 is the ferritic VSM figures of europium cation doping made from embodiment 1.
Embodiment
The present invention is made with reference to specific embodiment further to explain.
Raw material sources：Cabaltous nitrate hexahydrate：Purity AR, Chemical Reagent Co., Ltd., Sinopharm Group；Six nitric hydrate europiums：It is pure
Degree 99.9%, Aladdin chemical reagent Co., Ltd；Fe(NO3)39H2O：Purity AR, Chemical Reagent Co., Ltd., Sinopharm Group；
Sodium hydroxide：Purity AR, Chemical Reagent Co., Ltd., Sinopharm Group；Absolute ethyl alcohol：Purity AR, the comprehensive management of one factory of Shanghai reagent
Company.
Embodiment 1
A kind of europium doping Conjugate ferrite (Co0.8Eu0.2Fe2O4That is x=0.8) composite preparation method, method and step is such as
Under：
S1：1.6mmol Co (NO are sequentially added in 50mL deionized waters3)3·6H2O, 0.4mmol Eu (NO3)3·
6H2O and 4mmol Fe (NO3)3·9H2O, and stir, the NaOH solution that concentration is 5mol/L, regulation is added dropwise
PH value of solution persistently stirs 20min to 11.
S2：Solution is moved into reactor, isothermal reaction 10h at 180 DEG C；After the completion of reaction, solution is cooled to room temperature,
Precipitation is centrifuged repeatedly washing repeatedly to solution in neutrality with deionized water and ethanol.
S3：Finally 60 DEG C of dry 12h in vacuum drying chamber, produce x=0.8 Co0.8Eu0.2Fe2O4Europium adulterates ferro-cobalt oxygen
Composite material.
Embodiment 2
A kind of europium doping Conjugate ferrite (Co0.85Eu0.15Fe2O4That is x=0.85) composite preparation method, method step
It is rapid as follows：
S1：1.7mmol Co (NO are sequentially added in 50mL deionized waters3)3·6H2O, 0.3mmol Eu (NO3)3·
6H2O and 4mmol Fe (NO3)3·9H2O, and stir, the NaOH solution that concentration is 5mol/L, regulation is added dropwise
PH value of solution persistently stirs 20min to 11.5.
S2：Solution is moved into reactor, isothermal reaction 10h at 180 DEG C；After the completion of reaction, solution is cooled to room temperature,
Precipitation is centrifuged repeatedly washing repeatedly to solution in neutrality with deionized water and ethanol.
S3：Finally 60 DEG C of dry 12h in vacuum drying chamber, produce x=0.85 Co0.85Eu0.15Fe2O4Europium cation doping
Ferrite composite material.
Embodiment 3
A kind of europium doping Conjugate ferrite (Co0.9Eu0.1Fe2O4That is x=0.9) composite preparation method, method and step is such as
Under：
S1：1.8mmol Co (NO are sequentially added in 50mL deionized waters3)3·6H2O, 0.2mmol Eu (NO3)3·
6H2O and 4mmol Fe (NO3)3·9H2O, and stir, the NaOH solution that concentration is 5mol/L, regulation is added dropwise
PH value of solution persistently stirs 20min to 11.8.
S2：Solution is moved into reactor, isothermal reaction 10h at 180 DEG C；After the completion of reaction, solution is cooled to room temperature,
Precipitation is centrifuged repeatedly washing repeatedly to solution in neutrality with deionized water and ethanol.
S3：Finally 60 DEG C of dry 12h in vacuum drying chamber, produce x=0.9 Co0.9Eu0.1Fe2O4Europium adulterates ferro-cobalt oxygen
Composite material.
Embodiment 4
A kind of europium doping Conjugate ferrite (Co0.95Eu0.05Fe2O4That is x=0.95) composite preparation method, method step
It is rapid as follows：
S1：1.9mmol Co (NO are sequentially added in 50mL deionized waters3)3·6H2O, 0.1mmol Eu (NO3)3·
6H2O and 4mmol Fe (NO3)3·9H2O, and stir, the NaOH solution that concentration is 5mol/L, regulation is added dropwise
PH value of solution persistently stirs 20min to 12.
S2：Solution is moved into reactor, isothermal reaction 10h at 180 DEG C；After the completion of reaction, solution is cooled to room temperature,
Precipitation is centrifuged repeatedly washing repeatedly to solution in neutrality with deionized water and ethanol.
S3：Finally 60 DEG C of dry 12h in vacuum drying chamber, produce x=0.95 Co0.95Eu0.05Fe2O4Europium cation doping
Ferrite composite material.
Embodiment 5
A kind of europium doping Conjugate ferrite (Co0.8Eu0.2Fe2O4That is x=0.8) composite preparation method, method and step is such as
Under：
S1：1.6mmol Co (NO are sequentially added in 50mL deionized waters3)3·6H2O, 0.4mmol Eu (NO3)3·
6H2O and 4mmol Fe (NO3)3·9H2O, and stir, the NaOH solution that concentration is 3mol/L, regulation is added dropwise
PH value of solution persistently stirs 20min to 11.3.
S2：Solution is moved into reactor, isothermal reaction 10h at 180 DEG C；After the completion of reaction, solution is cooled to room temperature,
Precipitation is centrifuged repeatedly washing repeatedly to solution in neutrality with deionized water and ethanol.
S3：Finally 60 DEG C of dry 12h in vacuum drying chamber, produce x=0.8 Co0.8Eu0.2Fe2O4Europium adulterates ferro-cobalt oxygen
Composite material.
Embodiment 6
A kind of europium doping Conjugate ferrite (Co0.8Eu0.2Fe2O4That is x=0.8) composite preparation method, method and step is such as
Under：
S1：1.6mmol Co (NO are sequentially added in 50mL deionized waters3)3·6H2O, 0.4mmol Eu (NO3)3·
6H2O and 4mmol Fe (NO3)3·9H2O, and stir, the NaOH solution that concentration is 5mol/L, regulation is added dropwise
PH value of solution persistently stirs 20min to 11.2.
S2：Solution is moved into reactor, isothermal reaction 10h at 160 DEG C；After the completion of reaction, solution is cooled to room temperature,
Precipitation is centrifuged repeatedly washing repeatedly to solution in neutrality with deionized water and ethanol.
S3：Finally 60 DEG C of dry 12h in vacuum drying chamber, produce x=0.8 Co0.8Eu0.2Fe2O4Europium adulterates ferro-cobalt oxygen
Composite material.
Embodiment 7
A kind of europium doping Conjugate ferrite (Co0.8Eu0.2Fe2O4That is x=0.8) composite preparation method, method and step is such as
Under：
S1：1.6mmol Co (NO are sequentially added in 50mL deionized waters3)3·6H2O, 0.4mmol Eu (NO3)3·
6H2O and 4mmol Fe (NO3)3·9H2O, and stir, the NaOH solution that concentration is 5mol/L, regulation is added dropwise
PH value of solution persistently stirs 20min to 11.1.
S2：Solution is moved into reactor, isothermal reaction 12h at 180 DEG C；After the completion of reaction, solution is cooled to room temperature,
Precipitation is centrifuged repeatedly washing repeatedly to solution in neutrality with deionized water and ethanol.
S3：Finally 60 DEG C of dry 12h in vacuum drying chamber, produce x=0.8 Co0.8Eu0.2Fe2O4Europium adulterates ferro-cobalt oxygen
Composite material.
Accompanying drawing 1 is the XRD of embodiment 1, and the diffraction maximum at 2 θ=35.62 ° is higher relative to other appearances, peak intensity
And it is sharp, crystal growth degree of orientation height is represented, is more likely formed club shaped structure.
Accompanying drawing 2 is schemed for the TEM of embodiment 1, illustrates that obtained product is pure phase, the Co of Rod-like shape0.8Eu0.2Fe2O4Cobalt
Ferrite, its particle length are 1~1.8 μm, and draw ratio is 5~8.
Accompanying drawing 3 is the TEM figures of embodiment 2.Illustrate that obtained product is bar-like the Co of pattern0.85Eu0.15Fe2O4Ferro-cobalt
Oxysome, particle longest dimension is up to 2.5 μm.
Accompanying drawing 4 is schemed for the VSM of embodiment 1.Illustrate obtained product Co0.8Eu0.2Fe2O4The saturated magnetization of Conjugate ferrite
Intensity has a certain upgrade, and rare earth Eu doping has strengthened the magnetic moment of transition metal.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (9)
- A kind of 1. europium cation doping ferrite composite material, it is characterised in that chemical formula CoxEu1-xFe2O4, wherein x=0.80, 0.85,0.90,0.95.
- 2. a kind of europium cation doping ferrite composite material according to claim 1, it is characterised in that the composite is rod Shape structure.
- A kind of 3. preparation method of europium cation doping ferrite composite material according to claim 1, it is characterised in that method Step is as follows：S1：Europium nitrate, cobalt nitrate and ferric nitrate are sequentially added in deionized water, is stirred；Then NaOH is added dropwise Solution, the pH of solution is adjusted to alkalescence and continues to stir；S2:Solution obtained by S1 is moved into isothermal reaction in reactor.After the completion of reaction, solution is cooled to room temperature, spend from It is multiple that sub- water and ethanol will precipitate washing repeatedly；S3:Finally dry the product in vacuum drying chamber.
- 4. the preparation method of a kind of europium cation doping ferrite composite material according to claim 3, it is characterised in that described The metal salt sequentially added in S1 is six nitric hydrate europiums, cabaltous nitrate hexahydrate, Fe(NO3)39H2O.
- 5. the preparation method of a kind of europium cation doping ferrite composite material according to claim 4, it is characterised in that described Six nitric hydrate europiums, cabaltous nitrate hexahydrate, the amount of material of Fe(NO3)39H2O are 0.1-0.4:1.6-1.9:4.
- 6. the preparation method of a kind of europium cation doping ferrite composite material according to claim 3, it is characterised in that described The concentration of NaOH solution is 3-5mol/L in S1, and the pH value of solution is 10-12.
- 7. the preparation method of a kind of europium cation doping ferrite composite material according to claim 3, it is characterised in that described The reaction temperature of isothermal reaction kettle is 160-180 DEG C in S2, reaction time 10-12h.
- 8. the preparation method of a kind of europium cation doping ferrite composite material according to claim 3, it is characterised in that described Vacuum drying condition is that 12h is dried at 60 DEG C in S3.
- 9. europium cation doping ferrite composite material made from the preparation method according to claim any one of 3-8.
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| CN116813319A (en) * | 2023-05-24 | 2023-09-29 | 西北工业大学 | High-temperature dielectric wave-absorbing ceramic and preparation method thereof |
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| CN116813319A (en) * | 2023-05-24 | 2023-09-29 | 西北工业大学 | High-temperature dielectric wave-absorbing ceramic and preparation method thereof |
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