CN106587975A - Zinc ferrite material and preparation method thereof - Google Patents
Zinc ferrite material and preparation method thereof Download PDFInfo
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- CN106587975A CN106587975A CN201611240034.3A CN201611240034A CN106587975A CN 106587975 A CN106587975 A CN 106587975A CN 201611240034 A CN201611240034 A CN 201611240034A CN 106587975 A CN106587975 A CN 106587975A
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- 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
- C04B35/2658—Other ferrites containing manganese or zinc, e.g. Mn-Zn ferrites
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- 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
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- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
- H01F1/36—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites in the form of particles
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Abstract
The invention discloses a zinc ferrite material and a preparation method thereof, and belongs to the field of magnetic materials. The preparation method comprises the following steps of preparing materials, wherein raw materials comprise ferric acetylacetonate, zinc acetylacetonate, a surfactant and a solvent, the solvent is benzyl ether or 1-octadecene or oleylamine, the mole ratio of the zinc acetylacetonate to the ferric acetylacetonate is 0.1-0.8, the mole ratio of the total amount of the ferric acetylacetonate and the zinc acetylacetonate to the surfactant is 0.01-0.85, and the quantity of the solvent is determined in a manner that the ferric acetylacetonate and the zinc acetylacetonate can be fully dissolved by the solvent; placing the raw materials in protective gas environment, and performing uniform mixing at room temperature; and then performing low-speed warming, performing quick-speed warming, and performing cooling so as to obtain resultant granules namely the zinc ferrite material. The zinc ferrite material prepared by the method disclosed by the invention has extra-high saturation magnetization intensity, and can maintain favorable magnetic properties after being subjected to high temperature calcination.
Description
Technical field
The present invention relates to field of magnetic material, more particularly to a kind of Zinc ferrite material and preparation method thereof.
Background technology
Soft magnetic ferrite is the extremely wide magnetic functional material of a class application, in national defence, electronics, chemical industry, ceramics, biology
Have a wide range of applications with the multiple fields such as medical science.
The advantages of soft magnetic ferrite is generally configured with high magnetic permeability, high resistivity and low loss performance, saturation magnetization is made
For a key character parameter of soft magnetic ferrite, there is limit value to the magnetic conductivity and resonant frequency of material.It is existing
Soft magnetic ferrite, especially high-permeability material are often limited the application of material because saturation magnetization is low.Traditional soft
The ferritic saturation magnetization of magnet is usually 0.6T or lower, therefore ferrite as the frequency of high-permeability material application
Usually 1KHz to 10MHz.
As electronic device is to miniaturization and high frequency development, the operating frequency of soft magnetic ferrite is also badly in need of will be to
Ghz band develops, and the saturation magnetization of current soft magnetic ferrite can not meet needs, and current soft magnetic ferrite
The resistance to elevated temperatures of material can not meet the needs of development.
The content of the invention
It is an object of the invention to provide a kind of Zinc ferrite material and preparation method thereof.The Zinc ferrite material tool of the present invention
There is superelevation saturation magnetization, and good magnetic behavior can be kept after high-temperature calcination.
The purpose of the present invention is completed by following technical solution.
On the one hand, a kind of preparation method of Zinc ferrite material is embodiments provided, is comprised the steps：
Dispensing：Raw material includes ferric acetyl acetonade, zinc acetylacetonate, surfactant and solvent；Described solvent is dibenzyl
Ether or 1- octadecanes alkene or oleyl amine；
Wherein, the molar ratio 0.1～0.8 of zinc acetylacetonate and ferric acetyl acetonade, ferric acetyl acetonade and zinc acetylacetonate
The mol ratio of total amount and surfactant be 0.01～0.85, the amount of solvent can fully dissolve ferric acetyl acetonade and acetylacetone,2,4-pentanedione
Zinc；
Described raw material is placed in protective gas environment, normal temperature is mixed；Then Jing is heated up at a slow speed, is rapidly heated and cooled down
The composition granule that generates for obtaining afterwards is described Zinc ferrite material.
Further, described surfactant is the mixture or oleic acid or tristearin of oleic acid and 1,2- hexadecane diol
Acid.
Further, described intensification at a slow speed is that programming rate less than 5 DEG C/min is warmed up to 110～120 DEG C, and constant temperature is held
Continue more than 0.5h；
Described being rapidly heated is that programming rate higher than 7.5 DEG C/min is warmed up to 276-365 DEG C, and pyroreaction exceedes
20min。
Further, the described programming rate for heating up at a slow speed is 2-4 DEG C/min；
The described programming rate being rapidly heated as 10-15 DEG C/min is warmed up to temperature for 278-282 DEG C.
Further, the mol ratio of zinc acetylacetonate and ferric acetyl acetonade is 0.3～0.6；The ferric acetyl acetonade and second
The total amount of acyl acetone zinc is 0.4～0.6 with the mol ratio of surfactant；The consumption of described solvent is surfactant mole
3～20 times of amount.
Further, the consumption of described solvent is 5～12 times of surfactant mole.
Further, generation composition granule is cleaned with organic solvent, and is collected.
Further, described organic solvent is hexane, toluene, ethanol or methyl alcohol.
Second aspect, embodiments provides a kind of Zinc ferrite material, the chemistry of described Zinc ferrite material
Formula is：ZnXFe3-XO4；Wherein：0 ＜ X ＜ 0.53.
Further, described Zinc ferrite material is prepared by above-mentioned preparation method, the Zinc ferrite material
Normal temperature saturation magnetization is 90～120emu/g, and Curie temperature >=400 DEG C, material is calcined for 600-1200 DEG C under oxygen-free environment
Afterwards, normal temperature magnetic saturation magnetization reduces by 5% less than the magnetic saturation intensity of magnetization before calcining.
Compared with prior art, Zinc ferrite material of the present invention and preparation method thereof at least has the advantage that：
When filled a prescription by the Reasonable of ferric acetyl acetonade, zinc acetylacetonate and design the ratio of control ferro element and Zn-ef ficiency
Example；Simultaneously high temperature constant temperature guarantees that for a period of time air emptying and dissolution of raw material are fully in reaction unit for shielding gas emptying, further soon
Speed is warmed up to 280 DEG C, and oleic acid contributes to controlling ferro element in high-temperature reaction process as surfactant and Zn-ef ficiency is being given birth to
Distribution into the content in composition granule and in crystal structure, this is for its key effect of soft magnetic ferrite saturation magnetization.
Superelevation saturation magnetization high temperature resistant Zinc ferrite material of the present invention, compared with existing product, in saturation magnetic
Change and be greatly improved in intensity, and material still keeps good magnetic after the high-temperature calcination under oxygen-free environment
Can, the Curie temperature of the material is more than 400 DEG C.
Specific embodiment
For convenience of those skilled in the art's understanding to the present invention program, illustrate with reference to preferred embodiment,
It should be appreciated that preferred embodiment is to explain technical scheme, and not as the restriction of protection domain.
A kind of preparation method of Zinc ferrite material, comprises the steps：
Dispensing：Raw material includes ferric acetyl acetonade, zinc acetylacetonate, surfactant and solvent；Described solvent is dibenzyl
Ether or 1- octadecanes alkene or oleyl amine；
Wherein, the molar ratio 0.1～0.8 of zinc acetylacetonate and ferric acetyl acetonade, ferric acetyl acetonade and zinc acetylacetonate
The mol ratio of total amount and surfactant be 0.01～0.85, the amount of solvent can fully dissolve ferric acetyl acetonade and acetylacetone,2,4-pentanedione
Zinc；
Described raw material is placed in protective gas environment, normal temperature is mixed；Then Jing is heated up at a slow speed, is rapidly heated and cooled down
The composition granule that generates for obtaining afterwards is described Zinc ferrite material.
The chemical formula of Zinc ferrite material prepared by said method is：ZnXFe3-XO4；Wherein：0 ＜ X ＜ 0.53.
To note here is that：When filled a prescription by the Reasonable of ferric acetyl acetonade, zinc acetylacetonate and design control iron unit
The ratio of element and Zn-ef ficiency；Simultaneously high temperature constant temperature guarantees for a period of time air emptying and dissolution of raw material in reaction unit for shielding gas emptying
Fully, the species of shielding gas do not limited here, primarily to discharging air, prevents the composition in air from participating in reaction shadow
The preparation of Zinc ferrite material is rung, typically using gases such as argon gas, nitrogen, those skilled in the art can select as needed to close
Suitable shielding gas.
Above scheme can complete the preparation of Zinc ferrite material, and preferred version is given on this basis：
Preferably, described surfactant is the mixture or oleic acid or tristearin of oleic acid and 1,2- hexadecane diol
Acid.
To note here is that：Oleic acid contributes to controlling ferro element and zinc as surfactant in high-temperature reaction process
Content and distribution in crystal structure of the element in composition granule is generated, this is for its pass of soft magnetic ferrite saturation magnetization
Key is acted on.
Preferably, described intensification at a slow speed is the programming rate less than 5 DEG C/min is warmed up to 110～120 DEG C, constant temperature is held
Continue more than 0.5h；
Described being rapidly heated is that programming rate higher than 7.5 DEG C/min is warmed up to 276-365 DEG C, and pyroreaction exceedes
20min。
Preferably, the described programming rate for heating up at a slow speed is 2-4 DEG C/min；
The described programming rate being rapidly heated as 10-15 DEG C/min is warmed up to temperature for 278-282 DEG C.
To note here is that：The programming rate for heating up at a slow speed is controlled in 2-4 DEG C/min, is conducive to raw material to mix, dissolve
Fully, be conducive to draining air and vapor in reaction unit.
The programming rate being rapidly heated is 10-15 DEG C/min, is conducive to keeping uniformity of the crystal grain during growth,
The homogenization for being conducive to Zn ferrite particulate component and size is controlled.
Preferably, the mol ratio of zinc acetylacetonate and ferric acetyl acetonade is 0.3～0.6；The ferric acetyl acetonade and second
The total amount of acyl acetone zinc is 0.4～0.6 with the mol ratio of surfactant；The consumption of described solvent is surfactant mole
3～20 times of amount.
Preferably, the consumption of described solvent is 5～12 times of surfactant mole.
To note here is that：Surfactant plays a crucial role to the composition and crystal structure of Zn ferrite, and surface is lived
The reasonable volume of property agent advantageously forms the Zn ferrite particle of high saturation and magnetic intensity.
Preferably, cleaning generation composition granule with organic solvent, and collect.
Preferably, described organic solvent is hexane, toluene, ethanol or methyl alcohol.
To note here is that：Organic solvent is conducive to removing Zn ferrite granule surface activity agent of generation etc. in reaction
Additives, and to Zn ferrite particle without any destruction.
Embodiment 1
A kind of Zinc ferrite material and preparation method thereof, comprises the steps：
(1) dispensing
Ferric acetyl acetonade 12mmol, zinc acetylacetonate 2mmol, benzyl ether 20mL, oleic acid 28mmol.
(2) react
By the raw material in dispensing (1) in there-necked flask, temperature measuring equipment, air-breather, condensing unit and exhaust are connected
Device.
Stir 1h using magnetic force heater at normal temperatures.
At a slow speed (4 DEG C/min) are warmed up to 120 DEG C, and constant temperature continues 1h.
Quickly (16 DEG C/min) are warmed up to 280 DEG C, natural cooling after pyroreaction 0.5h.
Generation composition granule is cleaned with hexane, and is collected.
Performance test example：
Test object：Superelevation saturation magnetization high temperature resistant Zinc ferrite material, chemical formula described in embodiment 1：
Zn0.12Fe2.88O4。
Saturation magnetization is 94emu/g.
400 DEG C of Curie temperature.
After the high-temperature calcination 30min under 1200 DEG C of oxygen-free environments, the saturation magnetization of Zinc ferrite material is
92emu/g, after the high-temperature calcination 3h under 1200 DEG C of oxygen-free environments, the saturation magnetization of Zn ferrite is 90emu/g.
Embodiment 2：
(1) dispensing
Ferric acetyl acetonade 12mmol, zinc acetylacetonate 8.5mmol, benzyl ether 20mL, oleic acid 28mmol.
(2) react
A) by the raw material in dispensing (1) in there-necked flask, temperature measuring equipment, air-breather, condensing unit and row are connected
Device of air.
B) at normal temperatures using magnetic force heater stirring 1h.
C) at a slow speed (5 DEG C/min) are warmed up to 120 DEG C, and constant temperature continues 1h.
D) quick (16 DEG C/min) are warmed up to 280 DEG C, natural cooling after pyroreaction 0.5h.
E) generation composition granule is cleaned with toluene, and is collected.
Performance test example：
Test object：Superelevation saturation magnetization high temperature resistant Zinc ferrite material, chemical formula described in embodiment 2：
Zn0.48Fe2.52O4。
Saturation magnetization is 120emu/g.
402 DEG C of Curie temperature.
High saturation and magnetic intensity Zinc ferrite material after the high-temperature calcination 1h under 1200 DEG C of oxygen-free environments is
115emu/g。
Embodiment 3：
(1) dispensing
Ferric acetyl acetonade 12mmol, zinc acetylacetonate 10mmol, benzyl ether 20mL, oleic acid 28mmol.
(2) react
A) by the raw material in dispensing (1) in there-necked flask, temperature measuring equipment, air-breather, condensing unit and row are connected
Device of air.
B) at normal temperatures using magnetic force heater stirring 1h.
C) at a slow speed (5 DEG C/min) are warmed up to 110 DEG C, and constant temperature continues 1h.
D) quick (17 DEG C/min) are warmed up to 280 DEG C, natural cooling after pyroreaction 0.5h.
E) generation composition granule is cleaned with hexane, and is collected.
Performance test example：
Test object：Superelevation saturation magnetization high temperature resistant Zinc ferrite material, chemical formula described in embodiment 3：
Zn0.51Fe2.49O4。
Saturation magnetization is 104emu/g.
402 DEG C of Curie temperature.
High saturation and magnetic intensity Zinc ferrite material after the high-temperature calcination 1h under 1200 DEG C of oxygen-free environments is
100emu/g。
Raw material is commercially available prod described in embodiment 1-3, each component consumption is increased or decreased according to same ratio, gained
The parts by weight relation of each component belongs to protection scope of the present invention.
For the collection of product, those skilled in the art can as needed select hexane, toluene, ethanol or methyl alcohol etc.
Can be used for collecting the organic solvent of product of the present invention.
The present patent application most part, those skilled in the art according to existing knowledge and can be needed using existing conventional skill
Art specifically adopts which kind of reaction unit, here are not limited completing, such as.
The above, the only specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, any
Those familiar with the art the invention discloses technical scope in, change or replacement can be readily occurred in, all should contain
Cover within protection scope of the present invention.Therefore, protection scope of the present invention should be defined by the scope of the claims.
Claims (10)
1. a kind of preparation method of Zinc ferrite material, it is characterised in that comprise the steps：
Dispensing：Raw material includes ferric acetyl acetonade, zinc acetylacetonate, surfactant and solvent；Described solvent be benzyl ether or
1- octadecanes alkene or oleyl amine；
Wherein, the molar ratio 0.1～0.8 of zinc acetylacetonate and ferric acetyl acetonade, ferric acetyl acetonade and zinc acetylacetonate it is total
Amount is 0.01～0.85 with the mol ratio of surfactant, and the amount of solvent can fully dissolve ferric acetyl acetonade and zinc acetylacetonate；
Described raw material is placed in protective gas environment, normal temperature is mixed；Then obtain Jing after heating up at a slow speed, be rapidly heated and cool down
The composition granule that generates for arriving is described Zinc ferrite material.
2. the preparation method of Zinc ferrite material according to claim 1, it is characterised in that described surfactant is
The mixture or oleic acid or stearic acid of oleic acid and 1,2- hexadecane diol.
3. the preparation method of Zinc ferrite material according to claim 1, it is characterised in that described intensification at a slow speed is low
110～120 DEG C are warmed up in the programming rate of 5 DEG C/min, constant temperature is continued above 0.5h；
Described being rapidly heated is that programming rate higher than 7.5 DEG C/min is warmed up to 276-365 DEG C, and pyroreaction is more than 20min.
4. the preparation method of Zinc ferrite material according to claim 3, it is characterised in that the described liter for heating up at a slow speed
Warm speed is 2-4 DEG C/min；
The described programming rate being rapidly heated as 10-15 DEG C/min is warmed up to temperature for 278-282 DEG C.
5. the preparation method of Zinc ferrite material according to claim 1, it is characterised in that zinc acetylacetonate and levulinic
The mol ratio of ketone iron is 0.3～0.6；The total amount of the ferric acetyl acetonade and zinc acetylacetonate is with the mol ratio of surfactant
0.4～0.6；The consumption of described solvent is 3～20 times of surfactant mole.
6. the preparation method of Zinc ferrite material according to claim 5, it is characterised in that the consumption of described solvent is
5～12 times of surfactant mole.
7. the preparation method of Zinc ferrite material according to claim 1, it is characterised in that generation is cleaned with organic solvent
Composition granule, and collect.
8. the preparation method of Zinc ferrite material according to claim 7, it is characterised in that described organic solvent is for oneself
Alkane, toluene, ethanol or methyl alcohol.
9. a kind of Zinc ferrite material, it is characterised in that the chemical formula of described Zinc ferrite material is：ZnXFe3-XO4；Wherein：
0 ＜ X ＜ 0.53.
10. Zinc ferrite material according to claim 9, it is characterised in that described Zinc ferrite material will by right
Ask the preparation method described in any one of 1-8 to be prepared, the Zinc ferrite material normal temperature saturation magnetization be 90～
120emu/g, Curie temperature >=400 DEG C, under oxygen-free environment after 600-1200 DEG C of calcining, normal temperature saturation magnetization drops material
It is low less than 5% of the magnetic saturation intensity of magnetization before calcining.
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| CN109046369A (en) * | 2018-09-25 | 2018-12-21 | 安徽大学 | A kind of photochemical catalyst Sr2FeMoO6Preparation method |
| CN110408915A (en) * | 2018-04-27 | 2019-11-05 | 深圳大学 | A kind of spinel type ferrite film and preparation method thereof |
| CN111517369A (en) * | 2020-05-28 | 2020-08-11 | 中南大学 | Preparation method and application of iron-based bimetallic oxide nanocrystal |
| CN111732127A (en) * | 2020-07-02 | 2020-10-02 | 安徽大学 | Method for thermally synthesizing ferrite by magnetic field auxiliary solvent and method for regulating and controlling size and morphological characteristics of magnetic grains |
| CN113860756A (en) * | 2021-10-11 | 2021-12-31 | 西南科技大学 | Cobalt-titanium co-doped zinc ferrite film photo-anode material and preparation method and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110408915A (en) * | 2018-04-27 | 2019-11-05 | 深圳大学 | A kind of spinel type ferrite film and preparation method thereof |
| CN109046369A (en) * | 2018-09-25 | 2018-12-21 | 安徽大学 | A kind of photochemical catalyst Sr2FeMoO6Preparation method |
| CN111517369A (en) * | 2020-05-28 | 2020-08-11 | 中南大学 | Preparation method and application of iron-based bimetallic oxide nanocrystal |
| CN111517369B (en) * | 2020-05-28 | 2021-06-15 | 中南大学 | Preparation method and application of iron-based bimetallic oxide nanocrystal |
| CN111732127A (en) * | 2020-07-02 | 2020-10-02 | 安徽大学 | Method for thermally synthesizing ferrite by magnetic field auxiliary solvent and method for regulating and controlling size and morphological characteristics of magnetic grains |
| CN111732127B (en) * | 2020-07-02 | 2022-04-19 | 安徽大学 | Method for thermally synthesizing ferrite by magnetic field auxiliary solvent and method for regulating and controlling size and morphological characteristics of magnetic grains |
| CN113860756A (en) * | 2021-10-11 | 2021-12-31 | 西南科技大学 | Cobalt-titanium co-doped zinc ferrite film photo-anode material and preparation method and application thereof |
| CN113860756B (en) * | 2021-10-11 | 2023-01-24 | 西南科技大学 | Cobalt-titanium co-doped zinc ferrite film photo-anode material and preparation method and application thereof |
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