CN106518042A - Method for preparing spinel-type cerium-doped nano cobalt ferrite oxide - Google Patents
Method for preparing spinel-type cerium-doped nano cobalt ferrite oxide Download PDFInfo
- Publication number
- CN106518042A CN106518042A CN201611005822.4A CN201611005822A CN106518042A CN 106518042 A CN106518042 A CN 106518042A CN 201611005822 A CN201611005822 A CN 201611005822A CN 106518042 A CN106518042 A CN 106518042A
- Authority
- CN
- China
- Prior art keywords
- spinel
- cerium
- cobalt ferrite
- preparation
- mixes
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
- C04B35/2675—Other ferrites containing rare earth metals, e.g. rare earth ferrite garnets
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
- C04B35/2666—Other ferrites containing nickel, copper or cobalt
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention discloses a method for preparing spinel-type cerium-doped nano cobalt ferrite oxide. The method includes the steps that soluble saline solutions of metal cerium, cobalt and ferrum are mixed according to the stoichiometric ratio of CoFe2-xCexO4(x=0.1-0.4); citric acid is added according to the molar ratio of total metal ions in the CoFe2-xCexO4 to the citric acid being 1:1-3, and the pH value of the solution is adjusted to be 6.0-8.0; the warming and stirring reaction is carried out to obtain gel; and ignition is conducted after drying so that a self-propagating reaction can happen, and the spinel-type cerium-doped nano cobalt ferrite oxide can be obtained after constant temperature calcination of self-propagating reaction products. The nano CoFe2-xCexO4 ferrite prepared through the method is spinel structure cobalt ferrite with the high cerium doping amount and single crystalline phase. When the nano cobalt ferrite oxide is used as a wave-absorbing material, the dielectric loss and magnetic loss of the ferrite can be increased, the wave-absorbing capacity at the low-frequency stage is improved, and the absorbing frequency band is widened.
Description
Technical field
The present invention relates to a kind of ferritic preparation, the preparation method of more particularly to a kind of Conjugate ferrite mixed with cerium.
The ferrite for preparing in the process of the present invention has the spinel structure of single crystalline phase, and in low-frequency range (0～6GHz) with excellent
Absorbing property.
Background technology
In recent years, with the development of microwave technology, including radio telecommunications system, radar, microwave oven, mobile phone, medical treatment
The electromagnetic pollutions such as equipment cause the extensive concern of people, and many experts and scholar specially grind the research in this respect, to solve this
A little problems.Nanometer Cobalt Ferrite Oxide (CoFe2O4) it is a kind of excellent material of absorbing property, not only with higher coercivity, magnetocrystalline
Anisotropy, also with good saturation magnetization and larger magnetostriction, and has electronic isolation, chemical stability
The advantage of good and low cost.
But, single Conjugate ferrite is not wide enough in the suction wave frequency band of low-frequency range, and density is big, with the rising of temperature, its suction
Ripple performance can weaken.Numerous studies prove, by it is rare earth ion doped can be with the electromagnetic property of Effective Regulation Conjugate ferrite.Due to
Terres rares ion has not 4f electronics and strong Quantum geometrical phase angular momentum in pairs, therefore can improve the whole of Conjugate ferrite
Body electromagnetic performance, and then improve its absorbing property.
The preparation of rare earth doped Conjugate ferrite and performance are had been reported both at home and abroad.Journal of Materials
Processing Technology(2008, 98:39-46) report a kind of rare-earth Sm ion of sol-gel process synthesis to mix
Miscellaneous CoFe2O4Nanocrystal, the research show, as Sm ions dosages and temperature are from 400～1000 DEG C of increase, crystal grain
Magnetocrystalline anisotropy and distortion of lattice increase, cause the increase of its magnetic property.Rare Metal Materials and
Engineering (2012, 41(S3):The Dy doping Conjugate ferrites of collosol and gel self-assembly method synthesis are disclosed 523-526)
Magnetic Nano crystal grain, the research show that Dy doping causes the average grain size of cobalt ferrite nanoparticles to diminish, and with Dy
The increase of doping, sample coercivity substantially increase, and specific saturation magnetization declines.This two reports have all referred to rare earth unit
The plain impact of (Sm and Dy) to Nanometer Cobalt Ferrite Oxide magnetic property, but do not refer to the shadow of its absorbing property to Nanometer Cobalt Ferrite Oxide
Ring.
Aeronautical material journal (2016,36 (1):A kind of doping La is disclosed 48-52)3+'s
Ni0.35Co0.15Zn0.5LaxFe2O4The preparation method and absorbing property of absorbing material, the absorbing material 100～300nm of particle diameter, 1
In the range of～12GHz, when x=0.04, thickness of sample are maintained at 3mm or so, at the 9.8GHz maximum reflectivity reach-
16.49dB.But the particle diameter of the material is larger and little in the loss of low-frequency range (0～6GHz), reflectance is low, and absorbing property is poor.
Tianjin Normal University's journal (natural science edition) (2009,29 (1):One kind chemical coprecipitation is reported 36-38)
Nano Co Fe prepared by method2-xCexO4(x=0～0.3) powder body, its research show that, at cerium dopping amount x≤0.2, sample forms list
The one Conjugate ferrite phase with spinel structure, and then Conjugate ferrite phase and CeO during x ＞ 0.22Xiang Bingcun, and cerium dopping amount
There is stronger impact to the magnetic property of sample.Ceramics International(2014, 40:One is reported 5905-5911)
Plant the CoFe prepared with Sol-Gel auto-combustion method2-xCexO4(x=0,0.01,0.05,0.1,0.15) powder body, and point out cerium
Doping and sintering temperature are to affect CoFe2-xCexO4Two principal elements of infrared signature, CoFe1.95Ce0.05O4600
DEG C sintering 2h has a highest infrared emitting rate, when x ＞ 0.05, sintering temperature are higher than 600 DEG C, has the second crystalline phase CeO2Go out
It is existing.Ceramics International(2014, 40:CoFe prepared by a kind of molten-salt growth method is then reported 447-452)2- xCexO4(x=0,0.04,0.08) nano-powder, and impact of the doping of cerium to the quick characteristic of Conjugate ferrite gas propagated sensation is have studied, tie
Fruit shows as x=0.04, sensor is responded and running temperature affects maximum, have the second crystalline phase CeO during x=0.082Occur.Instrument
Table technology and sensor (2015, (5):CoFe prepared by a kind of spray heating decomposition is reported 14-16)2-xCexO4Nanometer
Crystal grain, which is uniformly applied to the alumina base plate surface with 2 gold electrodes using screen printing technique and forms sensitive thin film, if
A kind of film type acetone sensor is counted.With Ce3+Sensing element for sensitive thin film is capable of achieving acetone pollutant in vehicle exhaust
On-line checking, but have fluorite phase CeO as x=0.05 (i.e. the wt% of Ce be 3)2Diffraction maximum occurs, and with cerium dopping content
Increase, CeO2Characteristic diffraction peak gradually strengthens.
In the above-mentioned report with regard to mixing cerium cobalt ferrite material, Ce3+Doping all than relatively low, and with Ce3+Doping
Increase, all inevitably occur in that CeO2Second crystalline phase, it is impossible to form single spinel structure Conjugate ferrite phase.Together
When, these reports have also pertained only to mix impact of the cerium to Conjugate ferrite magnetic property and infrared signature, and sensing capabilities
Affect.Not yet it is related to mix the report of impact of the cerium to Conjugate ferrite absorbing property at present, especially at low-frequency range (0～6GHz)
Absorbing property.
The content of the invention
It is an object of the invention to provide a kind of spinel-type mixes the preparation method of cerium Nanometer Cobalt Ferrite Oxide, in the process of the present invention
Nano Co Fe of preparation2-xCexO4Ferrite has the spinel structure of higher cerium dopping amount and single crystalline phase, using which as suction
Wave material, can improve its absorbability in low-frequency range, widen absorption band.
To reach above-mentioned purpose, the present invention prepares nano Co Fe using following methods2-xCexO4Ferrite：
1) the soluble-salt aqueous solution of preparing metal cerium, cobalt and ferrum, by each aqueous solution and add citric acid obtain mixing it is molten
Liquid, wherein, the consumption of the soluble-salt of metallic cerium, cobalt and ferrum meets CoFe2-xCexO4Stoichiometric proportion, in the chemical formula
X=0.1～0.4, and CoFe2-xCexO4In total metal ion and the mol ratio of citric acid be 1: 1～3；
2) pH value for adjusting the mixed solution is 6.0～8.0, is warming up to 60～90 DEG C and is reacted, during reaction under stirring
The pH value for maintaining mixed solution is 6.0～8.0, obtains brown gel to reaction；
3) gel drying expansion is obtained into sepia xerogel, is crushed, add dehydrated alcohol, light generation self- propagating anti-
Should；
4) self-propagating reaction product obtains nano Co Fe of pitchy in 500～900 DEG C of calcining at constant temperature2-xCexO4Ferrite.
Wherein, described soluble-salt is nitrate, sulfate or hydrochlorate, present invention preferably uses nitrate.
It is highly preferred that the soluble-salt to be configured to the present invention aqueous solution that concentration is 0.2～0.5mol/L.
In the present invention, the citric acid can be directly added in the soluble-salt aqueous solution, it is also possible to by the lemon
Lemon acid is configured to aqueous solution with the soluble-salt aqueous solution.The concentration of the aqueous citric acid solution preferably 0.8～2mol/
L, more preferably 1.0mol/L.
The present invention adjusts the pH value of mixed solution using strong aqua ammonia.Usually, the mass fraction of the strong aqua ammonia is 25
～28%.
In the present invention, the dry expansion of the gel is carried out preferably in vacuum drying oven, and specifically the gel is existed
80～125 DEG C of 6～10h of dry expansion in vacuum drying oven.
Self-propagating reaction product is preferably risen to 500～900 DEG C with the heating rate of 10～20 DEG C/min by the present invention to be carried out
Calcining at constant temperature.
The time of the calcining at constant temperature is 1～4h.
With nano Co Fe prepared by said method of the present invention2-xCexO4Ferrite can improve which low as absorbing material
The absorbability of frequency range, widens absorption band.
By nano Co Fe for preparing2-xCexO4After ferrite wave-absorbing material grinding, using paraffin as binding agent, according to
Absorbing material: paraffin=6: 4 quality is rapidly injected the circle that thickness of sample is 3mm than mix homogeneously after 50～70 DEG C of consolutes
In cylindrical mold, the sample test absorbing property after solidification is taken.
Fig. 1 is given using the inventive method preparation doped with different proportion rare earth ion Ce3+CoFe2-xCexO4 (x
=0,0.1,0.2,0.3,0.4) suction wave profile in 0～6GHz frequency ranges.As seen from Figure 1, adulterate Ce3+It is purer afterwards
The absorbing property of Conjugate ferrite has large increase, and effective absorption band is widened, and its absworption peak is moved to low frequency range.Particularly
Work as Ce3+Doping be x=0.3 when, the minimum reflectance at frequency 5030MHz has reached -27.6dB, less than the frequency of -5dB
A width of 1.6GHz.
Rare earth ion Ce is prepared using the inventive method3+Doping Conjugate ferrite, has obtained Ce3+Doping is high, particle diameter is little,
The spinel nano CoFe of finely dispersed single crystalline phase2-xCexO4Powder body, the absorbing property of purer Conjugate ferrite have and carry greatly very much
Height, effective absorption band are widened, and its absworption peak is moved to low frequency range, has been widened the application of Conjugate ferrite, has been ferro-cobalt
Low-frequency range field application of the oxysome in terms of absorbing material opens wide prospect.
Description of the drawings
Fig. 1 is CoFe2-xCexO4(x=0,0.1,0.2,0.3,0.4) suction wave profile.
Fig. 2 is the X-ray diffraction analysis figure spectrum of different samples.
In figure, a is CoFe2O4, b is CoFe1.7Ce0.3O4。
Fig. 3 is the transmission electron microscope collection of illustrative plates of different samples.
In figure, a is CoFe1.7Ce0.3O4, b is CoFe2O4。
Specific embodiment
Following embodiments are only the preferred technical solution of the present invention, are not used to carry out any restriction to the present invention.For
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, made
Any modification, equivalent substitution and improvements etc., should be included within the scope of the present invention.
Embodiment 1
Weigh Co (NO3)2·6H2O、Fe(NO3)3·9H2O、Ce(NO3)3And citric acid, 0.3mol/L cobalt nitrates are configured to respectively
Solution, 0.3mol/L iron nitrate solutions, 0.3mol/L cerous nitrate solutions and 1.0mol/L citric acid solutions.Measure 20mL cobalt nitrates
Solution, 34mL iron nitrate solutions, 6mL cerous nitrate solutions and 54mL citric acid solutions are poured in 250mL beakers and are mixed, and stirring is lower slow
Slow Deca ammonia, adjusts the pH value of solution to 7.0.Reaction temperature is adjusted at 70 DEG C, the lower isothermal reaction of stirring is brown to solution
Gel, period adjust the pH value of a solution per half an hour, make to be maintained at 7.0.After reaction terminates, by gel reactant
It is transferred in crucible, is put in vacuum drying oven, in 100 DEG C of dry expansions 8h, obtains sepia xerogel.To expand in crucible
Xerogel smash to pieces, add a small amount of dehydrated alcohol to light, self-propagating reaction occur.Sample after self-propagating reaction is put into into Muffle furnace
In, 500 DEG C are risen to the heating rate of 15 DEG C/min, calcining at constant temperature 3h naturally cools to room temperature, obtains the nanometer of pitchy
CoFe1.7Ce0.3O4Absorbing material.
Comparative example 1
Weigh Co (NO3)2·6H2O、Fe(NO3)3·9H2O and citric acid, are configured to 0.3mol/L cobalt nitrate solutions, 0.3mol/L
Iron nitrate solution and 1.0mol/L citric acid solutions.Measure 20mL cobalt nitrate solutions, 40mL iron nitrate solutions and 54mL citric acids
Solution is poured in 250mL beakers and is mixed, and is slowly added dropwise ammonia under stirring, adjusts the pH value of solution to 7.0.Adjust reaction temperature to exist
70 DEG C, to the brown gel of solution, period adjusts the pH value of a solution to the lower isothermal reaction of stirring per half an hour, makes holding
7.0.After reaction terminates, gel reactant is transferred in crucible, is put in vacuum drying oven, in 100 DEG C of dry expansions
8h, obtains sepia xerogel.The xerogel expanded in crucible is smashed to pieces, is added a small amount of dehydrated alcohol to light, self- propagating is occurred
Reaction.Sample after self-propagating reaction is put in Muffle furnace, 500 DEG C is risen to the heating rate of 15 DEG C/min, calcining at constant temperature 3h,
Room temperature is naturally cooled to, nano Co Fe of pitchy is obtained2O4Absorbing material.
Fig. 2 gives embodiment 1 and comparative example 1 prepares the XRD spectrum of sample, and in figure, a and b are respectively CoFe2O4With
CoFe1.7Ce0.3O4。
From Fig. 2, curve a is can be seen that in 2 θ=18.2 °, 30.0 °, 35.4 °, 37.0 °, 43.0 °, 53.4 °, 56.9 °,
62.5 ° and 73.9 ° of characteristic absorption peak respectively with CoFe2O4(111), (220), (311), (222), (400), (422),
(511), (440) are corresponding with (533) crystallographic plane diffraction peak, and with PDF standard cards (ICDD-JCPDS 01-007-0426) completely
Unanimously, show that prepared sample is pure spinel structure CoFe2O4.From Fig. 1, curve b can be seen that CoFe1.7Ce0.3O4
Diffraction maximum peak position it is consistent with Conjugate ferrite peak position, illustrate Ce3+Mix the crystalline phase for affecting Conjugate ferrite, simply Ce3+Generation
For Fe3+Enter in ferritic lattice, do not occur mixing Ce3+Content increases the phenomenon for having the second crystalline phase to occur.But doping
Ce3+Conjugate ferrite diffraction peak intensity step-down, peak width broadens, and its reason is due to Ce3+Ratio of ionic radii Fe3+Ion half
Footpath is big, Ce3+Doping changes the structure of Conjugate ferrite after entering, cause crystal formation distortion, make grain growth imperfect, cause
Sample crystallinity is reduced.
Fig. 3 is TEM figures (a and b respectively nano Cos Fe of different samples1.7Ce0.3O4And CoFe2O4).Can be with from figure
Find out nano Co Fe1.7Ce0.3O4And CoFe2O4It is the particle diameter about finely dispersed ferrospinel of 60nm and 70nm respectively.
As a result show to mix Ce3+The particle diameter of Conjugate ferrite is little compared with pure Conjugate ferrite, and this is due to Ce3+During into lattice, spinelle can be replaced
In occupy the Fe of octahedral site3+, and Ce3+(1.02) radius is compared with Fe3+(0.67) radius is big, so working as Ce3+Replace
Fe3+When can cause lattice dilatation, and then result in distortion of lattice, the internal stress of generation causes the growth of the granule in solid state reaction
It is restricted, therefore, add the sample particle diameter of rare earth element to reduce.
Embodiment 2
Weigh Co (NO3)2·6H2O、Fe(NO3)3·9H2O、Ce(NO3)3And citric acid, 0.2mol/L cobalt nitrates are configured to respectively
Solution, 0.2mol/L iron nitrate solutions, 0.2mol/L cerous nitrate solutions and 1.0mol/L citric acid solutions.Measure 30mL cobalt nitrates
Solution, 54mL iron nitrate solutions, 6mL cerous nitrate solutions and 36mL citric acid solutions are poured in 250mL beakers and are mixed, and stirring is lower slow
Slow Deca ammonia, adjusts the pH value of solution to 8.0.Reaction temperature is adjusted at 60 DEG C, the lower isothermal reaction of stirring is brown to solution
Gel, period adjust the pH value of a solution per half an hour, make to be maintained at 8.0.After reaction terminates, by gel reactant
It is transferred in crucible, is put in vacuum drying oven, in 90 DEG C of dry expansions 9h, obtains sepia xerogel.To expand in crucible
Xerogel smash to pieces, add a small amount of dehydrated alcohol to light, self-propagating reaction occur.Sample after self-propagating reaction is put into into Muffle furnace
In, 600 DEG C are risen to the heating rate of 20 DEG C/min, calcining at constant temperature 2h naturally cools to room temperature, obtains the nanometer of pitchy
CoFe1.8Ce0.2O4Absorbing material.
Embodiment 3
Weigh Co (NO3)2·6H2O、Fe(NO3)3·9H2O、Ce(NO3)3And citric acid, 0.4mol/L cobalt nitrates are configured to respectively
Solution, 0.4mol/L iron nitrate solutions, 0.4mol/L cerous nitrate solutions and 1.0mol/L citric acid solutions.Measure 20mL cobalt nitrates
Solution, 32mL iron nitrate solutions, 8mL cerous nitrate solutions and 36mL citric acid solutions are poured in 250mL beakers and are mixed, and stirring is lower slow
Slow Deca ammonia, adjusts the pH value of solution to 5.0.Reaction temperature is adjusted at 60 DEG C, the lower isothermal reaction of stirring is brown to solution
Gel, period adjust the pH value of a solution per half an hour, make to be maintained at 5.0.After reaction terminates, by gel reactant
It is transferred in crucible, is put in vacuum drying oven, in 125 DEG C of dry expansions 7h, obtains sepia xerogel.To expand in crucible
Xerogel smash to pieces, add a small amount of dehydrated alcohol to light, self-propagating reaction occur.Sample after self-propagating reaction is put into into Muffle furnace
In, 750 DEG C are risen to the heating rate of 5 DEG C/min, calcining at constant temperature 4h naturally cools to room temperature, obtains the nanometer of pitchy
CoFe1.6Ce0.4O4Absorbing material.
Embodiment 4
Weigh Co (NO3)2·6H2O、Fe(NO3)3·9H2O、Ce(NO3)3And citric acid, 0.5mol/L cobalt nitrates are configured to respectively
Solution, 0.5mol/L iron nitrate solutions, 0.5mol/L cerous nitrate solutions and 1.0mol/L citric acid solutions.Measure 20mL cobalt nitrates
Solution, 38mL iron nitrate solutions, 2mL cerous nitrate solutions and 30mL citric acid solutions are poured in 250mL beakers and are mixed.Stirring is lower slow
Slow Deca ammonia, adjusts the pH value of solution to 6.0.Reaction temperature is adjusted at 60 DEG C, the lower isothermal reaction of stirring is brown to solution
Gel, period adjust the pH value of a solution per half an hour, make to be maintained at 6.0.After reaction terminates, by gel reactant
It is transferred in crucible, is put in vacuum drying oven, in 80 DEG C of dry expansions 6h, obtains sepia xerogel.To expand in crucible
Xerogel smash to pieces, add a small amount of dehydrated alcohol to light, self-propagating reaction occur.Sample after self-propagating reaction is put into into Muffle furnace
In, 500 DEG C are risen to the heating rate of 16 DEG C/min, calcining at constant temperature 1h naturally cools to room temperature, obtains the nanometer of pitchy
CoFe1.9Ce0.1O4Absorbing material.
Claims (10)
1. a kind of spinel-type mixes the preparation method of cerium Nanometer Cobalt Ferrite Oxide, the method comprising the steps of：
1) the soluble-salt aqueous solution of preparing metal cerium, cobalt and ferrum, by each aqueous solution and add citric acid obtain mixing it is molten
Liquid, wherein, the consumption of the soluble-salt of metallic cerium, cobalt and ferrum meets CoFe2-xCexO4Stoichiometric proportion, in the chemical formula
X=0.1～0.4, and CoFe2-xCexO4In total metal ion and the mol ratio of citric acid be 1: 1～3；
2) pH value for adjusting the mixed solution is 6.0～8.0, is warming up to 60～90 DEG C and is reacted, during reaction under stirring
The pH value for maintaining mixed solution is 6.0～8.0, obtains brown gel to reaction；
3) gel drying expansion is obtained into sepia xerogel, is crushed, add dehydrated alcohol, light generation self- propagating anti-
Should；
4) self-propagating reaction product obtains nano Co Fe in 500～900 DEG C of calcining at constant temperature2-xCexO4Ferrite.
2. spinel-type according to claim 1 mixes the preparation method of cerium Nanometer Cobalt Ferrite Oxide, it is characterized in that it is described can
Soluble is nitrate, sulfate or hydrochlorate.
3. spinel-type according to claim 1 mixes the preparation method of cerium Nanometer Cobalt Ferrite Oxide, it is characterized in that it is described can
Soluble is nitrate.
4. spinel-type according to claim 1 mixes the preparation method of cerium Nanometer Cobalt Ferrite Oxide, it is characterized in that described solvable
Property saline solution concentration be 0.2～0.5mol/L.
5. nano Co Fe according to claim 12-xCexO4Ferritic preparation method, is characterized in that the citric acid
It is configured to the aqueous solution and the soluble-salt aqueous solution of 0.8～2mol/L.
6. spinel-type according to claim 5 mixes the preparation method of cerium Nanometer Cobalt Ferrite Oxide, it is characterized in that the Fructus Citri Limoniae
The concentration of aqueous acid is 1.0mol/L.
7. spinel-type according to claim 1 mixes the preparation method of cerium Nanometer Cobalt Ferrite Oxide, and it is characterized in that will be described solidifying
Glue 80～125 DEG C of 6～10h of dry expansion in vacuum drying oven.
8. spinel-type according to claim 1 mixes the preparation method of cerium Nanometer Cobalt Ferrite Oxide, it is characterized in that self- propagating
Product rises to 500～900 DEG C with the heating rate of 10～20 DEG C/min and carries out calcining at constant temperature.
9. spinel-type according to claim 1 mixes the preparation method of cerium Nanometer Cobalt Ferrite Oxide, it is characterized in that the constant temperature
The time of calcining is 1～4h.
10. spinel-type according to claim 1 mixes the preparation method of cerium Nanometer Cobalt Ferrite Oxide, it is characterized in that use quality
Fraction is the pH value that 25～28% strong aqua ammonia adjust mixed solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611005822.4A CN106518042B (en) | 2016-11-16 | 2016-11-16 | A kind of spinel-type mixes the preparation method of cerium Nanometer Cobalt Ferrite Oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611005822.4A CN106518042B (en) | 2016-11-16 | 2016-11-16 | A kind of spinel-type mixes the preparation method of cerium Nanometer Cobalt Ferrite Oxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106518042A true CN106518042A (en) | 2017-03-22 |
| CN106518042B CN106518042B (en) | 2019-10-08 |
Family
ID=58353235
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611005822.4A Expired - Fee Related CN106518042B (en) | 2016-11-16 | 2016-11-16 | A kind of spinel-type mixes the preparation method of cerium Nanometer Cobalt Ferrite Oxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106518042B (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106976916A (en) * | 2017-04-17 | 2017-07-25 | 东南大学 | A kind of preparation method of high stability from carrier hydrogen-storing material |
| CN107416909A (en) * | 2017-08-28 | 2017-12-01 | 哈尔滨工业大学 | A kind of preparation method of iron-based oxide silica aerogel |
| CN109225264A (en) * | 2018-09-17 | 2019-01-18 | 齐齐哈尔大学 | The method of the preparation of gahnite modified catalyst and Catalytic Synthesis |
| CN110066598A (en) * | 2019-05-28 | 2019-07-30 | 河南嘉和节能科技有限公司 | A kind of high temperature anti-dropout infrared radiative energy-saving coating |
| CN113353987A (en) * | 2021-07-16 | 2021-09-07 | 中国科学院兰州化学物理研究所 | Spinel type ferrite material based on rare earth element lanthanum or cerium doping |
| CN114084910A (en) * | 2021-10-15 | 2022-02-25 | 闽都创新实验室 | Cerium-nickel-cobalt-doped ferrite nano material and preparation method and application thereof |
| CN114835169A (en) * | 2022-05-24 | 2022-08-02 | 沈阳理工大学 | Spinel type ferrite, preparation method thereof and wave-absorbing material |
| CN115925407A (en) * | 2022-05-25 | 2023-04-07 | 中国科学院赣江创新研究院 | Rare earth element doped Z-type ferrite material and preparation method thereof |
-
2016
- 2016-11-16 CN CN201611005822.4A patent/CN106518042B/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106976916A (en) * | 2017-04-17 | 2017-07-25 | 东南大学 | A kind of preparation method of high stability from carrier hydrogen-storing material |
| CN107416909A (en) * | 2017-08-28 | 2017-12-01 | 哈尔滨工业大学 | A kind of preparation method of iron-based oxide silica aerogel |
| CN109225264A (en) * | 2018-09-17 | 2019-01-18 | 齐齐哈尔大学 | The method of the preparation of gahnite modified catalyst and Catalytic Synthesis |
| CN110066598A (en) * | 2019-05-28 | 2019-07-30 | 河南嘉和节能科技有限公司 | A kind of high temperature anti-dropout infrared radiative energy-saving coating |
| CN113353987A (en) * | 2021-07-16 | 2021-09-07 | 中国科学院兰州化学物理研究所 | Spinel type ferrite material based on rare earth element lanthanum or cerium doping |
| CN113353987B (en) * | 2021-07-16 | 2023-10-31 | 中国科学院兰州化学物理研究所 | Spinel type ferrite material doped with rare earth element lanthanum or cerium |
| CN114084910A (en) * | 2021-10-15 | 2022-02-25 | 闽都创新实验室 | Cerium-nickel-cobalt-doped ferrite nano material and preparation method and application thereof |
| CN114084910B (en) * | 2021-10-15 | 2023-12-05 | 闽都创新实验室 | Cerium-nickel-cobalt doped ferrite nano material and preparation method and application thereof |
| CN114835169A (en) * | 2022-05-24 | 2022-08-02 | 沈阳理工大学 | Spinel type ferrite, preparation method thereof and wave-absorbing material |
| CN115925407A (en) * | 2022-05-25 | 2023-04-07 | 中国科学院赣江创新研究院 | Rare earth element doped Z-type ferrite material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106518042B (en) | 2019-10-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106518042B (en) | A kind of spinel-type mixes the preparation method of cerium Nanometer Cobalt Ferrite Oxide | |
| Vinnik et al. | Electromagnetic properties of zinc–nickel ferrites in the frequency range of 0.05–10 GHz | |
| Praveena et al. | Effect of Gd3+ on dielectric and magnetic properties of Y3Fe5O12 | |
| Kumar et al. | Cation distribution: a key to ascertain the magnetic interactions in a cobalt substituted Mg–Mn nanoferrite matrix | |
| Winiarska et al. | Manganese–zinc ferrite synthesis by the sol–gel autocombustion method. Effect of the precursor on the ferrite’s catalytic properties | |
| CN109762519B (en) | Preparation method of high-entropy alloy/oxide composite nano wave-absorbing material | |
| Sadhana et al. | Effect of Sm 3+ on dielectric and magnetic properties of Y 3 Fe 5 O 12 nanoparticles | |
| Bifa et al. | Magnetic properties of samarium and gadolinium co-doping Mn-Zn ferrites obtained by sol-gel auto-combustion method | |
| Mang et al. | Electromagnetic wave absorption properties of cobalt-zinc ferrite nanoparticles doped with rare earth elements | |
| Lin et al. | Structural and magnetic studies of Mg substituted cobalt composite oxide catalyst Co1− xMgxFe2O4 | |
| CN102260072A (en) | Method for synthesizing high-performance barium ferrite by using molten salt as flux and reaction medium | |
| Ye et al. | Development of (Zr, Mn) doped X-type hexaferrites for high frequency EMI shielding applications | |
| Lwin et al. | Influence of pH on the physical and electromagnetic properties of Mg–Mn ferrite synthesized by a solution combustion method | |
| Sawant et al. | The effect of Co substitution on the structural and magnetic properties of lithium ferrite synthesized by an autocombustion method | |
| Abhishek et al. | Structural and magnetic properties of Eu3+ substituted Mg-Cd nanoferrites: a detailed study of influence of high energy γ-rays irradiation | |
| CN103214037B (en) | Bar-shaped manganese-zinc ferrite magnetic material of a kind of self assembling type and preparation method thereof | |
| Tyagi et al. | Synthesis and characterization of SrFe 11.2 Zn 0.8 O 19 nanoparticles for enhanced microwave absorption | |
| Pei et al. | Effect of Bi-Co co-doping on the microstructure and magnetic properties of NiMgCuZn ferrites | |
| Awati et al. | Influence of Zn 2+ doping on the structural and surface morphological properties of nanocrystalline Ni-Cu spinel ferrite | |
| Bhuvaneshwari et al. | Influence of gadolinium doped in nickel nanoferrites on structural, optical, electrical, and magnetic properties | |
| Slimani et al. | Magnetic and microwave properties of Co0. 5Ni0. 5Fe2-xScxO4 (0.0≤ x≤ 0.1) nanosized spinel ferrites | |
| Babu et al. | Effect on structural and magnetic properties of aluminum substituted Ni–Zn nanoferrite system prepared via citrate-gel route | |
| Jiang et al. | Synthesis of polycrystalline CoFe2O4 and NiFe2O4 powders by auto-combustion method using a novel amino-based gel | |
| Lysenko et al. | TG, DSC, XRD, and SEM studies of the substituted lithium ferrite formation from milled Sm2O3/Fe2O3/Li2CO3 precursors | |
| CN104341152A (en) | Preparation method for garnet phase nano-powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20191008 Termination date: 20201116 |