CN108373327A - A kind of nickel zinc cerium soft magnetic ferrites and preparation method thereof - Google Patents
A kind of nickel zinc cerium soft magnetic ferrites and preparation method thereof Download PDFInfo
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- CN108373327A CN108373327A CN201810348410.3A CN201810348410A CN108373327A CN 108373327 A CN108373327 A CN 108373327A CN 201810348410 A CN201810348410 A CN 201810348410A CN 108373327 A CN108373327 A CN 108373327A
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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
- C04B35/2608—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead
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- 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
- C04B35/265—Compositions containing one or more ferrites of the group comprising manganese or zinc and one or more ferrites of the group comprising nickel, copper or cobalt
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- 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
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- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
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Abstract
The present invention discloses a kind of nickel zinc cerium soft magnetic ferrites and preparation method thereof, including following operating procedure, 1) stoichiometrically Ni0.4Zn0.6‑xCexFe2O4In deionized water by corresponding nickel nitrate, zinc nitrate, ferric nitrate dissolving, NiZnCe ferrite nano powders are prepared according to Sol-gel self- propagating powder methods；2) polyvinyl alcohol water solution by the NiZnCe ferrite nano powders addition a concentration of 6%-8% that step 1) obtains is granulated, the pellet of acquisition is pressed into loop sample, loop sample obtains NiZnCe soft magnetic ferrites in 950-1100 DEG C of 2-5h of heat preservation sintering.Ce is added in the nickel zinc cerium soft magnetic ferrites prepared in technical solution3+Ion, Ce3+Radius it is larger, the original ion distribution of nickel zinc ferrocerium oxysome is had an impact, the ferritic crystallite dimension of nickel zinc cerium is refined, initial permeability can reach 174, and Curie temperature is more than 330 DEG C, have good electromagnetic performance.
Description
Technical field
The present invention relates to soft magnetic ferrite technical fields, and in particular to a kind of nickel zinc cerium soft magnetic ferrites and its
Preparation method.
Background technology
Soft magnetic ferrite is widely used in each class of electronic devices such as communication, computer, power supply, is in electronic information industry
Very important basic function material, with the continuous improvement of electronic equipment precision and stability, current major part machine system
Because of small size demand, usual packaging density is very high, and there are apparent temperature gradient phenomenon, the parts of different parts for internal system
Environment temperature have larger difference, thus more stringent requirements are proposed to the temperature stability of Ferrite Material performance.Ferrite
The magnetic property of material depends not only on crystal structure, and the distribution feelings by microscopic appearance and magnetic ion in crystal structure
The influence of condition.
Existing NiZn Ferrite Materials lead to temperature stability because of reasons such as ion distribution, microstructure and crystal defects
Difference.
Based on this, study and design a kind of nickel zinc cerium soft magnetic ferrites and preparation method thereof.
Invention content
The technical problem to be solved by the present invention is to：Temperature stability is poor in use for existing Ferrite Material,
The material is caused to be applied to parts, the different temperatures of parts is asked in the environmental performance technologies such as differ greatly or even can not use
Topic, based on this kind of nickel zinc cerium soft magnetic ferrites of proposition and preparation method thereof, be added in the material component magnetism Ce from
Son, and the preparation method combined by using Sol-gel self- propagating powder the preparation methods and solid sintering technology, change its crystal knot
Structure, and then improve the temperature stability of the Ferrite Material prepared.
The present invention is achieved through the following technical solutions：
The general nominal formula of a kind of nickel zinc cerium soft magnetic ferrites, the nickel zinc cerium soft magnetic ferrites is
Ni0.4Zn0.6-xCexFe2O4, wherein 0 x≤0.20 ＜.
A kind of preparation method of nickel zinc cerium soft magnetic ferrites, including following operating procedure,
1) compound containing Ce, Ni, Zn, Fe is used, NiZnCe is prepared according to Sol-gel self- propagating powder methods
Ferrite nano powder；
2) polyvinyl alcohol of the NiZnCe ferrite nano powders addition a concentration of 6% -8% obtained step 1) is water-soluble
Liquid is granulated, and the pellet of acquisition is pressed into loop sample, loop sample is obtained in 950-1100 DEG C of 2-5h of heat preservation sintering
NiZnCe soft magnetic ferrites.
Wherein, NiZnCe is prepared using Sol-gel self- propagating powder methods in step 1) described in the step 1)
The specific method of ferrite nano powder is：In Ni0.4Zn0.6-xCexFe2O4It is 3 by the amount ratio of substance in deionized water solution：
1 is added citric acid, and sealing then in 3 hours of 90 DEG C of magnetic agitations, obtains brown-green precursor solution；By precursor solution
It is cooled to room temperature, PH to 7 is adjusted with ammonium hydroxide；The solution that pH value is 7 is dried at 95 DEG C and forms xerogel, finally by xerogel
Fluffy dendroid is generated by self-propagating combustion, NiZnCe ferrite nano powders are obtained after pulverizing.
By magnetic element ion Ce3+It is introduced into existing NiZn ferrite powders, rare earth ion Ce3+Radius it is larger, by
The influence of three-dimensional effect, Ce3+Octahedral site (B) will be preferentially entered.Ce3+4f electronic shell provide an ion magnetic moment,
Belong to magnetic ion.Ce3+It is enhanced into ferrite lattice by the influence to the original ion distribution of nickel zinc ferrocerium oxysome
The superexchange interaction of magnetic ion between tetrahedron (A) and octahedra (B), to improve the Curie temperature of material.
Magnetic element ion Ce is added3+Into NiZn ferrite nano powder preparation process, the ferrite prepared is received
Rice flour body has uniform component, minimum grain size, big specific surface area and high chemism, can additionally add not adding
Adding significantly reduces the sintering temperature of material under conditions of agent, and can refine the microcosmic crystallite dimension of Ferrite Material, improves iron oxygen
Compactness, the uniformity of body material improve the initial permeability and Curie temperature of material.
Below table is Ni0.4Zn0.6-xCexFe2O4Ferrite nano powder grain size (x values are different)：
1 Ni of table0.4Zn0.6-xCexFe2O4Ferrite nano powder grain size
The solid sintering technology used in the technical program, NiZnCe ferrite nano powders are by certain temperature and time
Sintering, can make NiZnCe Ferrite Materials crystal structure after molding more complete, and Ce ion distributions are more uniformly distributed, to one
Determine to improve the superexchange interaction between magnetic ion in degree, and then improves the Curie temperature of NiZnCe Ferrite Materials.
Sol-gel self-propagating powder preparation method combination solid sintering technology in the technical program, wherein sol-gel
Method is to prepare one of main method of nano-powder, which forms metal complex by complexing agent and metal ion, then
By being cross-linked to form high-molecular gel.In gel, the distribution of Ce uniform ions, during removing gelling agent by heat treatment,
Ce ions occur oxidation reaction and form nanometer oxide material.
Compound in the present invention as Ce, Ni, Zn, Fe of raw material, concretely chloride, nitrate, hydroxide,
Carbonate, acylate or alkoxide, these salt are dissolved into deionized water solution, and complex reaction life occurs with the citric acid of addition
The citrate of long corresponding metallic element, chelate of the citrate generated between metal ion and citrate,
Stability is very high.It ammonium hydroxide is being passed through in the reacting of the above compound of ferritic metallic element and citric acid adjusts PH containing forming
Value promotes the lemon of metal ion to alkalescent for neutrality its object is to consume the acid compound generated in reaction process
The carry out of acid complex reaction of formation is complete.
PH value is adjusted using ammonium hydroxide in the technical program, relative to the method for adjusting pH value using ammonia is passed through, is being operated
In without complicated aeration equipment and avoid snorkel from entering in solution causing the secondary pollution of prepared solution, reduce impurity or
Influence of the pollutant to material prescription accuracy, and then the consistency of material property is improved, the operation for being passed through ammonium hydroxide is used in addition,
The ammonia that can avoid volatilizing is endangered caused by human body or the pollution of environment.
Further, the concrete operation step of solid sintering process is in the step 2)：It is added a concentration of 6% -8%
Polyvinyl alcohol water solution is granulated so that nano-powder is bonded together, and prevents from cracking in forming process, by acquisition
Pellet is pressed into loop sample convenient for measuring the initial permeability of material, and loop sample is in 950-1100 DEG C of heat preservation sinterings 2-
5h makes ferrite nano powder that solid phase reaction further occur, and finally obtains NiZnCe ferrite soft magnetic block materials.
Further, in order to preferably realize the present invention, in the step 2), the specific method of compacting is, by NiZnCe
Nanometer pellet is pressed into loop sample with mold under 60MP pressure.
Further, in order to preferably realize the present invention, the specification of the NiZnCe nano-powders loop sample is Ф
12mm×Ф8mm×h5mm。
Further, in order to preferably realize the present invention, in the step 1), in being dissolved into deionized water, with analysis
Pure Ni (NO3)2·6H2O, Zn (NO3)2·6H2O, Ce (NO3)3·6H2O and Fe (NO3)3·9H2O is raw material, by chemical formula
Ni0.4Zn0.6-xCexFe2O4, 0 x≤0.20 ＜ carries out weighing dispensing.
The present invention has the advantage that and advantageous effect：
1) nickel zinc is prepared using Sol-gel self- propagating powder preparation method combination solid sintering technologies in the technical program
Cerium soft magnetic ferrites are prepared using the magnetic non magnetic ion of Ce ion substitutions with excellent electromagnetic performance and high Curie
The soft magnetic ferrite of temperature, has a wide range of applications scene.
2) Ce is added in the nickel zinc cerium soft magnetic ferrites prepared in the technical program3+Ion, Ce3+Radius compared with
Greatly, the original ion distribution of nickel zinc ferrocerium oxysome is had an impact, and refines the ferritic crystallite dimension of nickel zinc cerium, had good
Electromagnetic performance, by changing the microscopic appearance of material and being taken using magnetic ion in NiZn Ferrite Materials in the technical program
It can improve the electromagnetic performance of material for non magnetic ion and effectively improve the Curie temperature of material, therefore, utilize magnetic ion
The non magnetic ion in NiZn ferrites is replaced to prepare the soft magnetic ferrite material with excellent electromagnetic performance and high Curie temperature
Material, is with a wide range of applications.
Description of the drawings
Attached drawing described herein is used for providing further understanding the embodiment of the present invention, constitutes one of the application
Point, do not constitute the restriction to the embodiment of the present invention.In the accompanying drawings：
Fig. 1 is the X ray diffracting spectrum for the NiZnCe Ferrite Materials that embodiment 1-4 is prepared.
Specific implementation mode
To make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiment, the present invention is made
Further to be described in detail, exemplary embodiment of the invention and its explanation are only used for explaining the present invention, are not intended as to this
The restriction of invention.
Embodiment 1：
A kind of preparation method of nickel zinc cerium soft magnetic ferrites, including following operating procedure：
1) dispensing
To analyze pure Ni (NO3)2·6H2O, Zn (NO3)2·6H2O, Ce (NO3)3·6H2O and Fe (NO3)3·9H2O is original
Material, by chemical formula Ni0.4Zn0.55Ce0.05Fe2O4Carry out weighing dispensing；
2) it prepares
Stoichiometrically Ni0.4Zn0.55Ce0.05Fe2O4Nitrate dissolving is sufficiently mixed dissolving afterwards in deionized water
The solution of a concentration of 0.15mol/L is formed afterwards；The amount of citric acid and nitrate species is added than the lemon for 3 in the solution of preparation
Then acid seals, then 3 hours of magnetic agitation at 90 DEG C, obtain clear brown-green precursor solution；Precursor is molten
Ammonium hydroxide is added after being cooled to room temperature in liquid thereto again, its pH value is adjusted to 7；The solution that pH value is 7 is dried into formation at 95 DEG C
Xerogel is finally generated fluffy dendroid by xerogel by self-propagating combustion, and NiZnCe ferrite nanos are obtained after pulverizing
Powder；The NiZnCe ferrite nano powders of acquisition are added to a concentration of 8% polyvinyl alcohol water solution to be granulated；By gained
Pellet is pressed into loop sample (Ф 12mm × Ф 8mm × h5mm) with mold under 60MP pressure；By loop sample at 950 DEG C
Heat preservation sintering 5h obtains Ferrite Material.
The nickel zinc cerium soft magnetic ferrites that the present embodiment prepares, general formula are：Ni0.4Zn0.55Ce0.05Fe2O4,
In, x=0.05.
The nickel zinc cerium soft magnetic ferrites that the present embodiment prepares, Curie temperature are 208 DEG C, magnetic conductivity 124.
Embodiment 2：
A kind of preparation method of nickel zinc cerium soft magnetic ferrites, including following operating procedure：
1) dispensing
To analyze pure Ni (NO3)2·6H2O, Zn (NO3)2·6H2O, Ce (NO3)3·6H2O and Fe (NO3)3·9H2O is original
Material, by chemical formula Ni0.4Zn0.50Ce0.10Fe2O4Carry out weighing dispensing；
2) it prepares
Stoichiometrically Ni0.4Zn0.50Ce0.10Fe2O4After nitrate is dissolved in a certain amount of deionized water fully
The solution of a concentration of 0.15mol/L is formed after mixed dissolution；The solution of preparation is added to the amount ratio of citric acid and nitrate species
It for 3 citric acid, then seals, then 3 hours of magnetic agitation at 90 DEG C, obtains clear brown-green precursor solution；
Ammonium hydroxide is added after precursor solution is cooled to room temperature thereto again, its Ph value is adjusted to 7；By Ph values be 7 solution at 95 DEG C
Lower drying forms xerogel, and xerogel is finally generated fluffy dendroid by self-propagating combustion, NiZnCe is obtained after pulverizing
Ferrite nano powder；The nano-powder of acquisition is added to a concentration of 7% polyvinyl alcohol water solution to be granulated；By gained grain
Material is pressed into loop sample (Ф 12mm × Ф 8mm × h5mm) with mold under 60MP pressure；By loop sample at 1100 DEG C
Heat preservation sintering 3h obtains Ferrite Material.
The nickel zinc cerium soft magnetic ferrites that the present embodiment prepares, general formula are：Ni0.4Zn0.50Ce0.10Fe2O4,
In, x=0.10.
The nickel zinc cerium soft magnetic ferrites that the present embodiment prepares, Curie temperature are 238 DEG C, magnetic conductivity 140.
Embodiment 3：
A kind of preparation method of nickel zinc cerium soft magnetic ferrites, including following operating procedure：
1) dispensing
To analyze pure Ni (NO3)2·6H2O, Zn (NO3)2·6H2O, Ce (NO3)3·6H2O and Fe (NO3)3·9H2O is original
Material, by chemical formula Ni0.4Zn0.45Ce0.15Fe2O4Carry out weighing dispensing；
2) it prepares：
Stoichiometrically Ni0.4Zn0.45Ce0.15Fe2O4After nitrate is dissolved in a certain amount of deionized water fully
The solution of a concentration of 0.15mol/L is formed after mixed dissolution；The solution of preparation is added to the amount ratio of citric acid and nitrate species
It for 3 citric acid, then seals, then 3 hours of magnetic agitation at 90 DEG C, obtains clear brown-green precursor solution；
Ammonium hydroxide is added after precursor solution is cooled to room temperature thereto again, its Ph value is adjusted to 7；By Ph values be 7 solution at 95 DEG C
Lower drying forms xerogel, and xerogel is finally generated fluffy dendroid by self-propagating combustion, NiZnCe is obtained after pulverizing
Ferrite nano powder；The nano-powder of acquisition is added to a concentration of 6% polyvinyl alcohol water solution to be granulated；By gained grain
Material is pressed into loop sample (specification (Ф 12mm × Ф 8mm × h5mm) with mold under 60MP pressure；By loop sample 1000
2~5h of heat preservation sintering obtains Ferrite Material at DEG C.
The nickel zinc cerium soft magnetic ferrites that the present embodiment prepares, general formula are：Ni0.4Zn0.45Ce0.15Fe2O4,
In, x=0.15.
The nickel zinc cerium soft magnetic ferrites that the present embodiment prepares, chemical formula Ni0.4Zn0.45Ce0.15Fe2O4,
Curie temperature is 290 DEG C, magnetic conductivity 149.
Embodiment 4：
A kind of preparation method of nickel zinc cerium soft magnetic ferrites, including following operating procedure：
1) dispensing
To analyze pure Ni (NO3)2·6H2O, Zn (NO3)2·6H2O, Ce (NO3)3·6H2O and Fe (NO3)3·9H2O is original
Material, by chemical formula Ni0.4Zn0.40Ce0.20Fe2O4Carry out weighing dispensing；
2) it prepares
Stoichiometrically Ni0.4Zn0.40Ce0.20Fe2O4After nitrate is dissolved in a certain amount of deionized water fully
The solution of a concentration of 0.15mol/L is formed after mixed dissolution；The solution of preparation is added to the amount ratio of citric acid and nitrate species
It for 3 citric acid, then seals, then 3 hours of magnetic agitation at 90 DEG C, obtains clear brown-green precursor solution；
Ammonium hydroxide is added after precursor solution is cooled to room temperature thereto again, its Ph value is adjusted to 7；By Ph values be 7 solution at 95 DEG C
Lower drying forms xerogel, and xerogel is finally generated fluffy dendroid by self-propagating combustion, NiZnCe is obtained after pulverizing
Ferrite nano powder；The nano-powder of acquisition is added to a concentration of 7.5% polyvinyl alcohol water solution to be granulated；By gained
Pellet is pressed into loop sample with mold under 60MP pressure (specification is Ф 12mm × Ф 8mm × h5mm)；Loop sample is existed
Heat preservation sintering 3h obtains Ferrite Material at 1050 DEG C.
The nickel zinc cerium soft magnetic ferrites that the present embodiment prepares, chemical formula are：Ni0.4Zn0.40Ce0.20Fe2O4,
In, x=0.20, Curie temperature is 331 DEG C, magnetic conductivity 174.
The NiZnCe Ferrite Materials prepared in the present embodiment are sintered 3h at 1050 DEG C, measure the Ferrite Material
The curve that varies with temperature of magnetic conductivity it is as shown in Figure 1.When Ce contents are 0.20, initial permeability 174, Curie temperature
More than 330 DEG C.
The NiZnCe soft magnetic ferrite chemical general formulas that embodiment 1-4 prepares are Ni0.4Zn0.6-xCexFe2O4,
In, the magnetic conductivity of 0 x≤0.20 ＜, the material is 124-174, and Curie temperature is 238-331 DEG C.
Comparative example 1：
A kind of preparation method of nickel zinc cerium soft magnetic ferrites, including following operating procedure：
1) dispensing
To analyze pure Ni (NO3)2·6H2O, Zn (NO3)2·6H2O, Ce (NO3)3·6H2O and Fe (NO3)3·9H2O is original
Material, by chemical formula Ni0.4Zn0.6Fe2O4Carry out weighing dispensing；
2) it prepares
Stoichiometrically Ni0.4Zn0.6Fe2O4It is formed after nitrate dissolving is sufficiently mixed dissolving afterwards in deionized water
A concentration of 0.15molL-1Solution；The amounts of citric acid and nitrate species is added than the citric acid for 3 in the solution of preparation,
Then it seals, then 3 hours of magnetic agitation at 90 DEG C, obtains clear brown-green precursor solution；By precursor solution
Ammonium hydroxide is added after being cooled to room temperature thereto again, its Ph value is adjusted to 7；It is dry that the solution that Ph values are 7 is dried into formation at 95 DEG C
Xerogel is finally generated fluffy dendroid by gel by self-propagating combustion, and NiZnCe ferrite nano powder is obtained after pulverizing
Body；
The NiZnCe ferrite nano powders of acquisition are added to a concentration of 6% polyvinyl alcohol water solution to be granulated, it will
Gained pellet is pressed into loop sample with mold under 60MP pressure, and by loop sample, heat preservation sintering 2h obtains iron at 950 DEG C
Ferrite.
Wherein, the loop sample specification for suppressing acquisition is Ф 12mm × Ф 8mm × h5mm.
The nickel zinc cerium soft magnetic ferrites prepared in the present embodiment, general formula are：Ni0.4Zn0.6Fe2O4, wherein x=
0.00。
The nickel zinc cerium soft magnetic ferrites prepared in the present embodiment, Curie temperature are 187 DEG C, magnetic conductivity 120.
Embodiment 1-4 is compared with comparative example, by the way that Ce is added in embodiment 1-43+, original to nickel zinc ferrocerium oxysome
Ion distribution have an impact, change the ferritic crystal grain diameter of nickel zinc cerium, enhance nickel zinc cerium soft magnetic ferrites Curie
Temperature and magnetic conductivity.
Embodiment 1-4 prepares nickel zinc cerium soft magnetic ferrites, is applied in electronic product production, ferrite material
The temperature stability of material performance is not influenced by electronic product internal temperature gradient, substantially increases the temperature of different parts parts
Degree.
Above-described specific implementation mode has carried out further the purpose of the present invention, technical solution and advantageous effect
It is described in detail, it should be understood that the foregoing is merely the specific implementation mode of the present invention, is not intended to limit the present invention
Protection domain, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should all include
Within protection scope of the present invention.
Claims (7)
1. a kind of nickel zinc cerium soft magnetic ferrites, which is characterized in that the general nominal formula of the nickel zinc cerium soft magnetic ferrites
For Ni0.4Zn0.6-xCexFe2O4, wherein 0 x≤0.20 ＜.
2. a kind of a kind of preparation method of nickel zinc cerium soft magnetic ferrites described in claim 1, which is characterized in that including with
Lower operating procedure,
1) compound containing Ce, Ni, Zn, Fe is used, NiZnCe iron oxygen is prepared according to Sol-gel self- propagating powder methods
Body nano-powder；
2) the NiZnCe ferrite nanos powder that step 1) obtains is prepared into NiZnCe ferroxcubes according to solid sintering technology
Magnetic material.
3. a kind of preparation method of nickel zinc cerium soft magnetic ferrites according to claim 2, which is characterized in that the step
It is rapid 2) in the concrete operation step of solid sintering process be：A concentration of 6% -8% polyvinyl alcohol water solution is added to be granulated,
The pellet of acquisition is pressed into loop sample, loop sample obtains NiZnCe ferrites in 950-1100 DEG C of 2-5h of heat preservation sintering
Soft magnetic materials.
4. a kind of preparation method of nickel zinc cerium soft magnetic ferrites according to claim 2, which is characterized in that the step
It is rapid 1) in use Sol-gel self- propagating powder methods prepare the specific method of NiZnCe ferrite nano powders for：
Ni0.4Zn0.6-xCexFe2O4It is 3 by the amount ratio of substance in deionized water solution：1 is added citric acid, sealing, then in 90 DEG C of magnetic
Power stirs 3 hours, obtains brown-green precursor solution；Precursor solution is cooled to room temperature, PH to 7 is adjusted with ammonium hydroxide；It will
The solution that pH value is 7 is dried at 95 DEG C forms xerogel, and xerogel is finally generated fluffy dendroid by self-propagating combustion,
NiZnCe ferrite nano powders are obtained after pulverizing.
5. a kind of preparation method of nickel zinc cerium soft magnetic ferrites according to claim 3, which is characterized in that the step
It is rapid 2) in, the specific method of compacting is that NiZnCe nanometers of pellets are pressed into loop sample with mold under 60MP pressure.
6. a kind of preparation method of nickel zinc cerium soft magnetic ferrites according to claim 3, which is characterized in that described
The specification of NiZnCe nano-powder loop samples is Ф 12mm × Ф 8mm × h5mm.
7. a kind of preparation method of nickel zinc cerium soft magnetic ferrites according to claim 2, which is characterized in that the step
It is rapid 1) in, by dissolution of raw material in deionized water, to analyze pure Ni (NO3)2·6H2O, Zn (NO3)2·6H2O, Ce (NO3)3·
6H2O and Fe (NO3)3·9H2O is raw material, by chemical formula Ni0.4Zn0.6-xCexFe2O4, 0 x≤0.20 ＜ carries out weighing dispensing.
Priority Applications (1)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115367813A (en) * | 2022-08-16 | 2022-11-22 | 矿冶科技集团有限公司 | Spinel type nickel-zinc ferrite and preparation method and application thereof |
| CN115403366A (en) * | 2022-08-24 | 2022-11-29 | 厦门大学 | Lithium-doped nickel-zinc ferrite material and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0183988A2 (en) * | 1984-11-30 | 1986-06-11 | Kabushiki Kaisha Toshiba | Magnetic powders for magnetic recording media and magnetic recording media employing said magnetic powder therein |
| US20090261919A1 (en) * | 2007-10-24 | 2009-10-22 | Keycom Corporation | Millimeter wave band nonreciprocal device |
| CN101575206A (en) * | 2008-05-07 | 2009-11-11 | 重庆仪表材料研究所 | High-frequency high-power Ni-Zn base magnetic ferrite material and manufacturing method thereof |
| CN103467079A (en) * | 2013-08-28 | 2013-12-25 | 西北工业大学 | Preparation method for grapheme/Ni0.8Zn0.2Ce0.06Fe1.94O4 nano wave-absorbing material |
| CN104945759A (en) * | 2014-03-26 | 2015-09-30 | 深圳市润麒麟科技发展有限公司 | Cerium-doped nickel-zinc-ferrite-filled carbon nanotube composite wave-absorbing material and preparation thereof |
| CN106083024A (en) * | 2016-06-17 | 2016-11-09 | 盐城工学院 | A kind of cerium zinc is co-doped with NiFe2o4nano-powder and preparation method thereof |
-
2018
- 2018-04-18 CN CN201810348410.3A patent/CN108373327B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0183988A2 (en) * | 1984-11-30 | 1986-06-11 | Kabushiki Kaisha Toshiba | Magnetic powders for magnetic recording media and magnetic recording media employing said magnetic powder therein |
| US20090261919A1 (en) * | 2007-10-24 | 2009-10-22 | Keycom Corporation | Millimeter wave band nonreciprocal device |
| CN101575206A (en) * | 2008-05-07 | 2009-11-11 | 重庆仪表材料研究所 | High-frequency high-power Ni-Zn base magnetic ferrite material and manufacturing method thereof |
| CN103467079A (en) * | 2013-08-28 | 2013-12-25 | 西北工业大学 | Preparation method for grapheme/Ni0.8Zn0.2Ce0.06Fe1.94O4 nano wave-absorbing material |
| CN104945759A (en) * | 2014-03-26 | 2015-09-30 | 深圳市润麒麟科技发展有限公司 | Cerium-doped nickel-zinc-ferrite-filled carbon nanotube composite wave-absorbing material and preparation thereof |
| CN106083024A (en) * | 2016-06-17 | 2016-11-09 | 盐城工学院 | A kind of cerium zinc is co-doped with NiFe2o4nano-powder and preparation method thereof |
Non-Patent Citations (4)
| Title |
|---|
| URMAPATHY G等: "Influence of cerium substitution on structural, magnetic and dielectric properties of nanocrystalline Ni-Zn ferrites synthesized by combustion method", 《JOURNAL OF MATERIALS SCIENCE-MATERIALS IN ELECTRONICS》 * |
| 刘渊等: "铈离子掺杂镍基铁氧体的制备及其吸波性能", 《硅酸盐学报》 * |
| 夏德贵等: "《软磁铁氧体制造原理与技术》", 31 December 2010, 陕西科学技术出版社 * |
| 张川: "铁氧体基电磁波吸收材料的研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115367813A (en) * | 2022-08-16 | 2022-11-22 | 矿冶科技集团有限公司 | Spinel type nickel-zinc ferrite and preparation method and application thereof |
| CN115367813B (en) * | 2022-08-16 | 2023-11-24 | 矿冶科技集团有限公司 | Spinel type nickel zinc ferrite and preparation method and application thereof |
| CN115403366A (en) * | 2022-08-24 | 2022-11-29 | 厦门大学 | Lithium-doped nickel-zinc ferrite material and preparation method thereof |
| CN115403366B (en) * | 2022-08-24 | 2023-05-12 | 厦门大学 | Lithium-doped nickel-zinc ferrite material and preparation method thereof |
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