CN106396658B - A kind of method that solid phase reaction prepares spinel type ferrite material precursor - Google Patents
A kind of method that solid phase reaction prepares spinel type ferrite material precursor Download PDFInfo
- Publication number
- CN106396658B CN106396658B CN201610803107.9A CN201610803107A CN106396658B CN 106396658 B CN106396658 B CN 106396658B CN 201610803107 A CN201610803107 A CN 201610803107A CN 106396658 B CN106396658 B CN 106396658B
- Authority
- CN
- China
- Prior art keywords
- iron
- ferrite material
- material precursor
- spinel type
- type ferrite
- 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.)
- Active
Links
Images
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
- C04B35/2658—Other ferrites containing manganese or zinc, e.g. Mn-Zn ferrites
-
- 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
- C04B35/01—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
- C04B35/2683—Other ferrites containing alkaline earth metals or lead
-
- 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
- C04B35/64—Burning or sintering processes
- C04B35/65—Reaction sintering of free metal- or free silicon-containing compositions
-
- 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
- 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
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
-
- 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
- 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
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3213—Strontium oxides or oxide-forming salts thereof
-
- 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
- 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
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3215—Barium oxides or oxide-forming salts thereof
-
- 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
- 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
- C04B2235/40—Metallic constituents or additives not added as binding phase
- C04B2235/405—Iron group metals
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/76—Crystal structural characteristics, e.g. symmetry
- C04B2235/762—Cubic symmetry, e.g. beta-SiC
- C04B2235/763—Spinel structure AB2O4
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention discloses a kind of method that solid phase reaction prepares spinel type ferrite material precursor, for this method by after iron oxide powder and iron powder and blended metal oxide powder mixing and ball milling, agglomeration, drying, the dry block merging of gained contain CO and CO2In mixed atmosphere, roasted at a temperature of being not higher than 1200 DEG C to get spinel type ferrite material precursor；This method is compared with the method for traditional high-temperature roasting method synthetic spinel material, maturing temperature is low, the time is short, substantially reduce calcining time and the requirement to equipment, avoid the use of the additives such as fluxing agent, the product purity of acquisition is high, and simple production process, it is at low cost, be conducive to industrialized production.
Description
Technical field
The present invention relates to a kind of preparation method of ferrospinel material precursor, in particular to a kind of solid phase reaction system
The method of standby spinel type ferrite material precursor, belongs to the preparation field of spinel type ferrite material.
Background technique
Ferrite is primarily referred to as the composite oxides of iron and other one or more kinds of metallic elements, according to crystal structure
Difference, be broadly divided into spinel-type, carbuncle type, Magnetoplumbate-type (hexangle type), Ca-Ti ore type, ilmenite type, NaCl type,
Seven kinds of rutile-type.Wherein spinel type ferrite property is stable, have excellent magnetic characteristics, preparation process is relatively easy, is to find most
Early, transformer battery core, filter magnetic core and magnetic note are prepared frequently as soft magnetic material using most a kind of ferrites
Record element etc.；Furthermore spinel type ferrite is alternatively arranged as absorbing material, is used to prepare electromagnetic radiation physical protection, communication drop
It makes an uproar, the fields such as Information Security and military weapon stealth material.
Ferrospinel (MFe2O4) in M be primarily referred to as atomic radius and Fe2+Close bivalent metal ion (nickel,
Manganese, zinc, magnesium, barium, strontium etc.).In the crystal structure of ferrospinel, oxonium ion presses cubic close stacked arrangement, divalent sun
Ion is filled in eighth tetrahedron gap, and ferric ion is filled in the octahedral interstices of half.
Preparing the main method of spinel type ferrite material at present includes high-temperature solid phase reaction method and wet chemical methods.
Wet chemical methods include coprecipitation, solution-gel method, hydrothermal synthesis method etc..Its cardinal principle is in solubility
Metal salt under solution system, require distribution to be set to uniform solution according to target group, then by changing the items such as pH value of solution
Part converts precipitating etc. for the hydroxyl groups precursors of composite metal salt, finally by washing of precipitate, drying, roasting, can be obtained target
Product.Wet chemical methods can obtain property stabilization, even-grained ferrite product, still, process flow complexity, yield
Low defect causes such method that can not be widely used in actual industrial production.
Sintering process is the main method of current industrial production Ferrite Material, first by ingredient, is accurately controlled various
The content and ratio of metal oxide guarantee former using ball milling, mixing, drying and one section or multistage sintering process
Expect the solid phase reaction process of intermediate ion diffusion, due to raw material poor activity, solid phase reaction rate is low, therefore, general in production to burn
Range of the junction temperature at 1000 DEG C -1500 DEG C, needs calcining time long.In actual production, to reduce sintering time and temperature,
A small amount of fluxing agent is often added, this aspect can introduce impurity, on the other hand cause partial melting to generate sintering liquid phase, after being unfavorable for
Continuous working process.The advantages of sintering process is simple process, is convenient for large-scale production, but not due to raw material solid phase oxide active
Height, and need long-time ball milling to guarantee uniformity, cause sintering process to prepare unstable product quality.Fluxing agent mainly includes
CaO、SiO2、Nb2O5、V2O5、Bi2O3、MoO3、TiO2, one of CuO etc. or several combinations, dosage be generally molar ratio
1% hereinafter, dosage and ratio must be strictly controlled, otherwise can seriously affect ferrite product performance indicator.
Therefore, develop a kind of low temperature, efficiently, the process for preparing spinel type ferrite of environmental protection, can delay significantly
Solution China's Ferrite Material production capacity is insufficient, still needs to the status of a large amount of imports.
Summary of the invention
Deficiency existing for spinel technology is prepared for existing high temperature oxidation roasting, the purpose of the present invention is be
A kind of method for the preparation high-purity spinel type ferrite material precursor that maturing temperature is low, the time is short is provided.
In order to achieve the above technical purposes, before preparing spinel type ferrite material the present invention provides a kind of solid phase reaction
The method for driving body, this method are by after iron oxide powder and iron powder and blended metal oxide powder mixing and ball milling, and agglomeration is done
Dry, the dry block of gained is placed in containing CO and CO2In mixed atmosphere, roasted at a temperature of 800~1200 DEG C to get spinelle
Type ferrite material precursor.
Technical solution of the present invention prepares ferrospinel material primarily directed to traditional high-temperature solid phase reaction method
It improves.Traditional high-temperature solid phase reaction method mainly utilizes in pyroprocess, the solid phase between metal oxide and ferriferous oxide
Reaction, and temperature is the main reason of control element diffusion, therefore, needs to improve by improving maturing temperature in production
Reaction rate, or a small amount of fluxing agent of addition etc. improve Ion transfer speed, but excessively high maturing temperature and fluxing agent makes
It is generated with will lead to a small amount of liquid phase, partial melting is unfavorable for the subsequent processing to product, can also reduce properties of product.Of the invention
Technical solution key is that using the atmosphere combination metal iron powder containing CO uses, and under the common activation of the two, makes iron
Oxide is in the state of activation, is not only advantageous to accelerate reaction rate, and the metal oxide for being also beneficial to doping is easier to enter
In the lattice of magnetic iron ore spinelle, replace the iron ion of divalent；Meanwhile accelerate ferrous ion migration velocity, to synthesizing
Cheng Youli.By acting synergistically above, the use for reducing maturing temperature, reducing fluxing agent may be implemented, improve combined coefficient
And product purity.
Preferred scheme, the blended metal oxide powder mole are iron total moles in iron oxide powder and iron powder
The 10~50% of amount.
Preferred scheme, iron powder mole are within the 15% of iron oxide powder mole.
More preferably scheme, iron oxide powder include ferric oxide powder and/or ferroferric oxide powder.
More preferably scheme, blended metal oxide powder include nickel oxide, manganese oxide, zinc oxide, magnesia, oxidation
At least one of barium, strontium oxide strontia powder.
Preferred scheme contains CO and CO2Mixed atmosphere includes following volumes percent composition: CO 1~15.5%；CO 2 40
~84.5%；N2≤ 50% (0~50%).
Preferred scheme, the time of the roasting are 1~3h.
Preferred scheme is less than -0.045mm by the granularity 100% of ball mill grinding to mixed material.
Preferred scheme, product of roasting are cooled to room temperature under protective atmosphere.The protective atmosphere refers generally to nitrogen
Gas or inert gas and their combination.Such as N2And/or Ar.
Compared with the prior art, technical solution of the present invention bring advantageous effects:
1) technical solution of the present invention biggest advantage is that greatly reducing solid phase reaction prepares spinel type ferrite
The temperature of material precursor, shortens the reaction time, changes reaction condition mildly, achievees the purpose that energy conservation, reduces cost.And show
There is sintering temperature in technology to be up to the range within 1500 DEG C, and calcining time is long, to reduce sintering time and temperature, often adds
Add a small amount of fluxing agent, on the one hand cosolvent can introduce impurity, on the other hand cause partial melting to generate sintering liquid phase, after being unfavorable for
Continuous working process.And in technical solution of the present invention, it has suffered temperature in synthesis process and controls at 1200 DEG C hereinafter, generated time contracts
It is as short as 60~180min, and does not need to add the additive of other impure ingredients, production efficiency is substantially increased, is conducive to work
Industry metaplasia produces.
2) the spinel type ferrite material precursor purity is high of technical solution of the present invention preparation, crystal structure are uniformly steady
It is fixed, it is used directly for preparing ferrite product.Overcome the spinel type ferrite material forerunner of conventional solid method synthesis
Body there are uniformities it is poor, crystal structure is uneven the problems such as.
Detailed description of the invention
[Fig. 1] is the product XRD spectrum of embodiment 1.
[Fig. 2] is the product XRD spectrum of comparative example 1.
Specific embodiment
Following embodiment is intended to further illustrate the content of present invention, rather than limits the protection model of the claims in the present invention
It encloses.
Embodiment 1
Di-iron trioxide, metal iron powder, zinc oxide are subjected to ingredient, wherein metal iron powder accounts for the ratio of iron-bearing material and is
15mol%, the ratio that zinc oxide accounts for iron-bearing material is 50mol%, raw material is milled to after mixing to granularity 100%
Less than -0.045mm.Then it adds 10% water and 0.3% CMC organic binder carries out agglomeration, agglomerate drying is placed on
15.5%CO-84.5%CO2It in the mixed gas of composition, roasts 1.5 hours, will be taken out after sample cooling at 1000 DEG C
Franklinite ferrite material material precursor is obtained, product is through XRD quantitative analysis it is found that spinelle content is 98.7%.This
The ferrospinel XRD analysis obtained under part as shown in Figure 1, the diffraction maximum for the ZnO not dissociated in map, illustrate substantially with
Ferriferous oxide fully reacting, into the lattice of spinelle.
Comparative example 1
Di-iron trioxide, metal iron powder, zinc oxide are subjected to ingredient, wherein metal iron powder accounts for the ratio of iron-bearing material and is
15mol%, the ratio that zinc oxide accounts for iron-bearing material is 50mol%, raw material is carried out after mixing be milled to granularity 100% small
In -0.045mm.Then it adds 10% water and 0.3% CMC organic binder carries out agglomeration, agglomerate drying is placed on lazy
Property atmosphere in, roasted 1.5 hours at 1000 DEG C, will sample it is cooling after take out, before can be obtained franklinite Ferrite Material
Body is driven, product is through XRD quantitative analysis it is found that spinelle content is 78.7%.The ferrospinel XRD obtained under this condition points
Analysis has the diffraction maximum of largely free ZnO as shown in Figure 1, in map, illustrates that sample unreacted is complete.
Embodiment 2
Ferroso-ferric oxide, metal iron powder, manganese oxide are subjected to ingredient, wherein metal iron powder accounts for the ratio of iron-bearing material and is
10mol%, the ratio that manganese oxide accounts for iron-bearing material is 20mol%, raw material is carried out after mixing be milled to granularity 100% small
In -0.045mm.Then it adds 9.5% water and 0.2% CMC organic binder carries out agglomeration, agglomerate drying is placed on
1.0%CO-80%CO2- 19%N2It in the mixed gas of composition, roasts 1 hour, will be taken out after sample cooling at 1200 DEG C
Jakobsite ferrite material material precursor is obtained, product is through XRD quantitative analysis it is found that spinelle content is 99.7%.
Embodiment 3
Di-iron trioxide, metal iron powder, zinc oxide, manganese oxide are subjected to ingredient, wherein manganese oxide accounts for the ratio of iron-bearing material
Example is 10mol%, and it is 15mol% that zinc oxide, which accounts for iron-bearing material ratio, and raw material is carried out after mixing to be milled to granularity 100%
Less than -0.045mm.Then it adds 9.5% water and 0.2% CMC organic binder carries out agglomeration, agglomerate drying is placed on
10.5%CO-74.5%CO2- 15%N2It in the mixed gas of composition, roasts 2 hours, will be taken out after sample cooling at 1100 DEG C,
It can be obtained MnZn hercynite ferrite material material precursor, product is through XRD quantitative analysis it is found that spinelle content is
98.6%.
Embodiment 4
Ferroso-ferric oxide, di-iron trioxide, metal iron powder, manganese oxide are subjected to ingredient, wherein ferroso-ferric oxide, three oxidations
The ratio that two iron, metal iron powder account for iron-bearing material is respectively 40mol%, 50mol%, 10mol%, and wherein manganese oxide accounts for iron content original
The ratio of material is 10mol%, and raw material is carried out to being milled to granularity 100% after mixing less than -0.045mm.Then it adds
9.7% water and 0.4% CMC organic binder carry out agglomeration, by agglomerate drying be placed on 10%CO-40%CO2- 50%N2
It in the mixed gas of composition, is roasted 3 hours at 800 DEG C, will be taken out after sample cooling, can be obtained jakobsite ferrite material
Material precursor, product is through XRD quantitative analysis it is found that spinelle content is 98.1%.
Embodiment 5
Ferroso-ferric oxide, di-iron trioxide, metal iron powder, magnesia are subjected to ingredient, wherein ferroso-ferric oxide, three oxidations
The ratio that two iron, metal iron powder account for iron-bearing material is respectively 20mol%, 70mol%, 10mol, and wherein magnesia accounts for iron-bearing material
Ratio be 10mol%, magnesia account for iron-bearing material ratio be 10mol%, raw material is carried out after mixing to be milled to granularity
100% is less than -0.045mm.Then it adds 9.7% water and 0.4% CMC organic binder carries out agglomeration, agglomerate is dry
It is placed on 10%CO-70%CO2- 20%N2It in the mixed gas of composition, roasts 3 hours, will be taken out after sample cooling at 900 DEG C,
It can be obtained magnoferrite ferrite material material precursor, product is through XRD quantitative analysis it is found that spinelle content is 99.0%.
Embodiment 6
Ferroso-ferric oxide, di-iron trioxide, metal iron powder, nickel oxide are subjected to ingredient, wherein ferroso-ferric oxide, three oxidations
The ratio that two iron, metal iron powder account for iron-bearing material is respectively 80mol%, 15mol%, 5mol%, and wherein nickel oxide accounts for iron content original
The ratio of material is 20mol%, and raw material is carried out to being milled to granularity 100% after mixing less than -0.045mm.Then it adds
9.7% water and 0.4% CMC organic binder carry out agglomeration, by agglomerate drying be placed on 12%CO-58%CO2- 30%N2
It in the mixed gas of composition, is roasted 2.2 hours at 1050 DEG C, will be taken out after sample cooling, can be obtained NiFe_2O_4 spinel iron oxygen
Body material precursor, product is through XRD quantitative analysis it is found that spinelle content is 98.6%.
Embodiment 7
Ferroso-ferric oxide, metal iron powder, barium monoxide are subjected to ingredient, wherein ferroso-ferric oxide, metal iron powder account for iron content original
The ratio of material is respectively 85mol%, 15mol%, and the ratio that wherein barium monoxide accounts for iron-bearing material is 28mol%, and raw material is mixed
Carry out being milled to granularity 100% after uniformly less than -0.045mm.Then 9.7% water and 0.4% CMC organic binder are added
Agglomeration is carried out, agglomerate drying is placed on 3.5%CO-46.5%CO2- 50%N2In the mixed gas of composition, roasted at 1150 DEG C
1.5 hours, it will be taken out after sample cooling, can be obtained barium hercynite ferrite material material precursor, product is through XRD quantitative analysis
It is found that spinelle content is 98.8%.
Embodiment 8
Ferroso-ferric oxide, metal iron powder, barium monoxide, strontium oxide strontia are subjected to ingredient, wherein ferroso-ferric oxide, metal iron powder account for
The ratio of iron-bearing material is respectively 90mol%, 10mol%, and it is 18mol%, oxidation that wherein barium monoxide, which accounts for the ratio of iron-bearing material,
The ratio that strontium accounts for iron-bearing material is 8mol%, and raw material is carried out to being milled to granularity 100% after mixing less than -0.045mm.So
9.7% water is added afterwards and 0.4% CMC organic binder carries out agglomeration, and agglomerate drying is placed on 5.5%CO-74.5%
CO2- 20%N2It in the mixed gas of composition, is roasted 1.7 hours at 1100 DEG C, will be taken out after sample cooling, can be obtained barium iron point
Spar ferrite material material precursor, product is through XRD quantitative analysis it is found that spinelle content is 98.6%.
Claims (5)
1. a kind of method that solid phase reaction prepares spinel type ferrite material precursor, it is characterised in that: by ferriferous oxide powder
After end and iron powder and blended metal oxide powder mixing and ball milling, agglomeration, drying, the dry block merging of gained contain CO and CO2It is mixed
It closes in atmosphere, carries out 1~3h of roasting at a temperature of 800~1200 DEG C to get spinel type ferrite material precursor；
The iron powder mole is within the 15% of iron oxide powder mole；
Described contains CO and CO2Mixed atmosphere includes following volumes percent composition:
CO 1~15.5%；
CO240~84.5%；
N2≤ 50%.
2. the method that solid phase reaction according to claim 1 prepares spinel type ferrite material precursor, feature exist
In: the blended metal oxide powder mole is 10~50% of iron integral molar quantity in iron oxide powder and iron powder.
3. the method that solid phase reaction according to claim 1 or 2 prepares spinel type ferrite material precursor, feature
Be: the iron oxide powder includes ferric oxide powder and/or ferroferric oxide powder.
4. according to right want 1 or 2 described in the solid phase reaction method for preparing spinel type ferrite material precursor, feature exists
In: the blended metal oxide powder include nickel oxide, manganese oxide, zinc oxide, magnesia, barium monoxide, in strontium oxide strontia
At least one powder.
5. the method that solid phase reaction according to claim 1 or 2 prepares spinel type ferrite material precursor, feature
Be: the granularity 100% of the ball mill grinding to mixed material is less than 0.045mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610803107.9A CN106396658B (en) | 2016-09-05 | 2016-09-05 | A kind of method that solid phase reaction prepares spinel type ferrite material precursor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610803107.9A CN106396658B (en) | 2016-09-05 | 2016-09-05 | A kind of method that solid phase reaction prepares spinel type ferrite material precursor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106396658A CN106396658A (en) | 2017-02-15 |
| CN106396658B true CN106396658B (en) | 2019-10-15 |
Family
ID=57998684
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610803107.9A Active CN106396658B (en) | 2016-09-05 | 2016-09-05 | A kind of method that solid phase reaction prepares spinel type ferrite material precursor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106396658B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108640669A (en) * | 2018-06-20 | 2018-10-12 | 陕西理工大学 | A kind of high performance ferrite magnetic material and preparation method thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102503388A (en) * | 2011-09-21 | 2012-06-20 | 景德镇陶瓷学院 | Method for reducing firing shrinkage of strontium ferrite magnetic material, and product prepared by method |
| CN102992753A (en) * | 2012-11-23 | 2013-03-27 | 天长市昭田磁电科技有限公司 | Low power consumption preparation method of Mn-Zn soft magnetic ferrite material |
| CN102992752A (en) * | 2012-11-23 | 2013-03-27 | 天长市昭田磁电科技有限公司 | Method for preparing manganese-zinc (MnZn) soft magnetic ferrite |
| CN105060874A (en) * | 2015-08-10 | 2015-11-18 | 天长市昭田磁电科技有限公司 | Manganese zinc ferrite material for increasing electrical resistivity |
| CN105097172A (en) * | 2015-08-10 | 2015-11-25 | 天长市昭田磁电科技有限公司 | Low-magnetic-loss ferrite core material |
| CN105330280A (en) * | 2015-11-27 | 2016-02-17 | 全椒君鸿软磁材料有限公司 | Preparation method of high-impedance soft magnetic ferrite core material |
| CN105330283A (en) * | 2015-11-27 | 2016-02-17 | 全椒君鸿软磁材料有限公司 | Preparation method of high-frequency high-DC (Direct Current) superposition soft magnetic ferrite core material |
-
2016
- 2016-09-05 CN CN201610803107.9A patent/CN106396658B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102503388A (en) * | 2011-09-21 | 2012-06-20 | 景德镇陶瓷学院 | Method for reducing firing shrinkage of strontium ferrite magnetic material, and product prepared by method |
| CN102992753A (en) * | 2012-11-23 | 2013-03-27 | 天长市昭田磁电科技有限公司 | Low power consumption preparation method of Mn-Zn soft magnetic ferrite material |
| CN102992752A (en) * | 2012-11-23 | 2013-03-27 | 天长市昭田磁电科技有限公司 | Method for preparing manganese-zinc (MnZn) soft magnetic ferrite |
| CN105060874A (en) * | 2015-08-10 | 2015-11-18 | 天长市昭田磁电科技有限公司 | Manganese zinc ferrite material for increasing electrical resistivity |
| CN105097172A (en) * | 2015-08-10 | 2015-11-25 | 天长市昭田磁电科技有限公司 | Low-magnetic-loss ferrite core material |
| CN105330280A (en) * | 2015-11-27 | 2016-02-17 | 全椒君鸿软磁材料有限公司 | Preparation method of high-impedance soft magnetic ferrite core material |
| CN105330283A (en) * | 2015-11-27 | 2016-02-17 | 全椒君鸿软磁材料有限公司 | Preparation method of high-frequency high-DC (Direct Current) superposition soft magnetic ferrite core material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106396658A (en) | 2017-02-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101404197B (en) | Manganese zinc soft magnetic ferrite and production method for its magnetic core | |
| CN105565790A (en) | YR950 wide-temperature high-direct-current-superposition low-power-consumption manganese-zinc ferrite material and preparation method thereof | |
| CN103058643B (en) | Mn-Zn soft magnetic ferrite material with high, temperature, high superposition and low power consumption, and preparation method of Mn-Zn soft magnetic ferrite material | |
| CN113372108B (en) | Preparation method of high-entropy ceramic material with good light absorption performance | |
| CN103113093A (en) | High-frequency and high-impedance manganese zinc ferrite bead and production method thereof | |
| CN103613368B (en) | A kind of Aluminum oxide pure black ceramic material | |
| CN113087515B (en) | Manganese zinc ferrite with high saturation magnetic induction intensity, wide temperature range and low magnetic core loss, preparation method thereof and application of potassium tetrafluoroaluminate | |
| CN113087516B (en) | Low-temperature sintering method for preparing manganese-zinc ferrite by using industrial wastes | |
| CN101640090A (en) | High performance soft magnetic ferrite materials doped with Ni-Zn series and preparation method thereof | |
| CN112430081B (en) | High-saturation-flux-density soft magnetic ferrite material and preparation method thereof | |
| CN113698192A (en) | Method for preparing permanent magnetic ferrite by taking ultrapure magnetite concentrate as raw material | |
| CN102367209A (en) | Oxide-doped medium-low temperature mixed conducting oxygen-permeable membrane material and its preparation method | |
| CN103848620B (en) | LiMnZn ferrite material and preparation method thereof | |
| CN106396658B (en) | A kind of method that solid phase reaction prepares spinel type ferrite material precursor | |
| CN103159469A (en) | Preparation method of Mn-Zn ferrite powder with high permeability | |
| EP0127427B1 (en) | Production of microcrystralline ferrimagnetic spinels | |
| CN106882956A (en) | A kind of ceramic material and its processing method | |
| CN100554165C (en) | A kind of method of trimanganese tetroxide preparation | |
| CN115677337B (en) | Power ferrite material and preparation method and application thereof | |
| CN107555483B (en) | A kind of preparation method of jakobsite magnetic material presoma | |
| CN102898129B (en) | La-Zn co-doping permanent magnetic strontium ferrite material powder and preparation method thereof | |
| KR970008749B1 (en) | Process for the preparation of nickel-zinc ferrite powder | |
| CN106431379A (en) | Method for preparing Sn-Fe spinel material through low-temperature solid-phase reaction | |
| CN106887587A (en) | The stability lithium manganate battery electrode material and preparation method of a kind of glass fluxing technique | |
| US5626788A (en) | Production of magnetic oxide powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |