CN106498497A - A kind of method for preparing granule single crystallization Co2Z hexad ferrite powder body - Google Patents
A kind of method for preparing granule single crystallization Co2Z hexad ferrite powder body Download PDFInfo
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- CN106498497A CN106498497A CN201610850897.6A CN201610850897A CN106498497A CN 106498497 A CN106498497 A CN 106498497A CN 201610850897 A CN201610850897 A CN 201610850897A CN 106498497 A CN106498497 A CN 106498497A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
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- C30B29/22—Complex oxides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
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Abstract
The invention discloses one kind prepares high purity granular single crystallization Co2The method of Z-type ferrite powder, is that initiation material passes through to optimize compound precipitantses consumption and its feed postition with soluble metallic salt so that metallic element is uniformly distributed in presoma powder body；Further, presoma is mixed with salt, in heat treatment process, using fused salt liquid phase as ion transmission medium, accelerate metal ion diffusion in heat treatment process, promote target product to be formed, and by liquid growth, promote target product granular grows to tend to Growth Habit, assume single crystallization.The method is from technique relative to preparation Co2Z hexad ferrite conventional methods have more preferable phase control power, and can realize the single crystallization of granule from grain structure, are Co2Z hexad ferrites correlation high-performance electronic components and parts design and development is ensured there is provided high-quality powder body.
Description
Technical field
The present invention relates to a kind of coprecipitation prepares the Co of granule single crystallization2The method of Z hexad ferrite powder body,
Belong to the advanced synthesis field of functional material.
Background technology
Complex oxide Co2Z hexad ferrites as typical high-frequency soft magnetic material, because which is imitated in electricity, magnetic and magnetic-electricity
Should etc. aspect characteristic, especially initial permeability is high, resonant frequency is high, quality factor are high, heat stability is good, it is low excellent to be lost
Point so as to exist in microwave antenna, magnetic-optic devicess etc. and be widely applied.In order to meet the demand and high-performance of device design
Change, synthesize pure phase Co2Z hexad ferrites, and its grain structure is control effectively is premise.However, on chemically constituting
From the point of view of, Co2Z hexad ferrite chemical compositions are generally Ba3-xSrxCo2Fe24O41, relatively complicated；From crystal packing structure
On, Co2It is increasingly complex in common M types or Y type hexad ferrite crystal packing structures that Z hexad ferrites are compared, and this causes
Composition precise control is realized in building-up process, obtains high-purity Co2Z hexad ferrite relative difficulties.This situation is mixed in element
Become even more complicated under miscellaneous situation.Further, Co2Z hexad ferrite granule monocrystalline turns to its application, further improving performance
New approach is provided, but this technical method obtains high-purity target Co relative to mutually being formed from control thing2Z hexad ferrites
Just more difficult.
At present, common synthesis Co2The method of Z hexad ferrites is mainly solid reaction process, one side solid phase synthesis process
Final product is frequently accompanied by the presence of other types ferrous oxide impurity；On the other hand the difficulty for particle size with pattern has
Control, not to mention be to realize granule single crystallization.For this purpose, exploitation is applied to complex oxide Co2Z hexad ferrite high purity granulars
The Preparation Technique of Powders of single crystallization is for the great meaning of the good application of such material.
Content of the invention
The present invention is intended to provide one kind prepares high purity granular single crystallization Co2The method of Z-type ferrite powder.
Realization the technical scheme is that：One kind prepares high purity granular single crystallization Co2The method of Z-type ferrite powder,
It is that initiation material passes through to optimize compound precipitantses consumption and its feed postition with soluble metallic salt so that metallic element is in forerunner
It is uniformly distributed in body powder body；Further, presoma is mixed with salt, in heat treatment process, is transmitted as ion using fused salt liquid phase
Medium, accelerates metal ion diffusion in heat treatment process, promotes target product to be formed, and by liquid growth, promotes target to produce
Composition granule growth tends to Growth Habit, assumes single crystallization.Its specific implementation step is as follows：
1) according to Co2Z hexad ferrite chemical formula Ba3-xSrxCo2Fe24O41, x=0-3, weigh barium, strontium, cobalt, ferrum element can
Soluble metal salts is dissolved in deionized water, obtains mixed salt solution, and wherein, iron concentration is 0.5～3.0 mol/L,
Other concentration of metal ions are according to stoichiometric proportion；
2) mixture with alkali and carbonate is dissolved in deionized water, obtains compound precipitantses molten as compound precipitantses
Liquid；
3）Under agitation, composite precipitation agent solution is added step 1 with certain drop speed）In the metal salt solution；Continue
Stirring reaction is until reaction system ionic strength remains stable；
4）By step 3）Serosity after coprecipitation reaction carries out centrifugal treating, removes the centrifugation supernatant, and centrifugal deposition is through super
Sound is scattered in deionized water again through centrifugation, is cleaned repeatedly, is close to neutrality to centrifugal clear liquid；
5）Gained is centrifuged product and dries to constant weight at 60～90 DEG C, and obtains presoma powder body through grinding to crush；
6）With salt-mixture as disperse medium, mix by gained presoma powder body and by mechanical ball milling with disperse medium
Even, then heat treatment is carried out, obtain synthetic product；
7）Synthetic product is ground, and adds 70～90 DEG C of hot water to clean repeatedly, remove salt medium, through 70～90 DEG C
Drying obtains target ferrite powder product.
Step 1）In, described soluble metallic salt is chlorate or nitrate.
Step 2）In, described alkali is sodium hydroxide, potassium hydroxide or ammonia；Described carbonate is sodium carbonate, carbonic acid
Potassium or ammonium carbonate, in the preferred sodium hydroxide-sodium carbonate of described compound precipitantses, potassium hydroxide-potassium carbonate and ammonia-ammonium carbonate
Any one.
Step 2）In, in composite precipitation agent solution alkali concn be 1.0～5.0 mol/L, carbonate concentration be 0.01～
0.10 mol/L.
Step 3）In, the alkali consumption in compound precipitantses is the amount of the amount with 2 times of cobalt ion materials of 3 times of iron ion materials
The 100%～150% of summation, carbonate consumption are the 100%～150% of barium ionss and the amount summation of strontium ion material.
Step 3）In, the drop speed control of composite precipitation agent solution stirs speed between 2～20 ml/ minutes during Deca
Rate is 100～600 revs/min；The stirring reaction time is 12～48 hours.
Step 4）In, centrifugal treating rotating speed is 2000～10000 revs/min, and the centrifugal treating time is 5～30 minutes.
Step 6）In, described disperse medium using any two kinds in sodium chloride, potassium chloride, sodium sulfate and potassium sulfate or its
Thing mixed above, in mixture, the mol ratio of each material is 1:1；The consumption of disperse medium for precursor weight 30% ~
400%.
Step 6）In, in mechanical ball milling, ratio of grinding media to material is 10:1～5:1, ball milling speed is 100～400 revs/min, during ball milling
Between be 1～8 hour.
Step 6）In, the heating rate of heat treatment is 2～10 DEG C/min, and heat treatment process is to be incubated 30 at 400 DEG C
Minute～2 hours, be continuously heating to 1～4 hour is incubated at 1000 DEG C, then it is little to be warming up to insulation 4～12 at 1150～1300 DEG C
When.
Compared with prior art, the invention has the beneficial effects as follows：
1st, the present invention combines co-precipitation and fused salt technology, is to solve Co2Z hexad ferrite thing phases purity is asked with grain structure control
Topic, design are adapted to synthesis particle single crystallization Co2The method of Z hexad ferrite powder body；
2nd, the method by compound precipitantses selection, consumption and adds rate controlled, realizes that metallic element is equal in coprecipitation process
Even mixing, and then, used by heat treatment temperature system and fused salt in heat treatment process, based on fused salt liquid phase, promote thing phase
Formation and the single crystallization of granule；
3rd, the method from technique relative to prepare Co2Z hexad ferrite conventional methods have more preferable phase control power, and
The single crystallization of granule can be realized from grain structure, be Co2Z hexad ferrites correlation high-performance electronic components and parts design and development
Ensure there is provided high-quality powder body；
4th, the present invention is directed to Co2Z hexad ferrites chemical composition and crystal structure are complicated, be difficult to the complex oxide material that synthesizes
Synthesis, can also be that the control of the synthesis of other similar complex oxides and grain structure provide the reference in method.
Description of the drawings
Fig. 1 synthesizes Co2Z-type hexad ferrite (Ba1.5Sr1.5Co2Fe24O41) powder body X ray diffracting spectrum.
Fig. 2 synthesizes Co2Z-type hexad ferrite (Ba1.5Sr1.5Co2Fe24O41) powder body stereoscan photograph.
Fig. 3 synthesizes Co2Z-type hexad ferrite (Ba1.5Sr1.5Co2Fe24O41) powder body VSM curves.
Fig. 4 synthesizes Co2Z-type hexad ferrite (Ba3Co2Fe24O41) powder body X ray diffracting spectrum.
Fig. 5 synthesizes Co2Z-type hexad ferrite (Ba3Co2Fe24O41) powder body stereoscan photograph.
Fig. 6 synthesizes Co2Z-type hexad ferrite (Ba3Co2Fe24O41) powder body VSM curves.
Fig. 7 synthesizes Co2Z-type hexad ferrite (Sr3Co2Fe24O41) powder body X ray diffracting spectrum.
Fig. 8 synthesizes Co2Z-type hexad ferrite (Sr3Co2Fe24O41) powder body stereoscan photograph.
Fig. 9 synthesizes Co2Z-type hexad ferrite (Sr3Co2Fe24O41) powder body VSM curves.
Specific embodiment
Co around granule single crystallization2The preparation of Z hexad ferrite powder body, the present invention devise co-precipitation-fused salt knot
The technology of conjunction, passes through to add the process conditions such as speed for compound precipitantses species with consumption, precipitant in coprecipitation process
Preferred, obtain the uniform presoma powder body of starting metals Elemental redistribution；Further with salt-mixture for disperse medium, at heat
Science and engineering skill parameter coordination, plays molten salt system metal ion diffusion in heat treatment process is accelerated, promotes target product to be formed, and
By liquid growth, promote target product granular grows to tend to Growth Habit, assume single crystallization.The method can achieve Co2Z
The prepartion of hexad ferrite complex oxide and the control of grain structure, also can carry for synthesizing other oxidase complex objects systems
For using for reference.
Case study on implementation 1：
With chemical composition as Ba1.5Sr1.5Co2Fe24O41Co2As a example by Z hexad ferrites：Soluble metal halogenide is selected, is pressed
Weigh according to stoichiometric proportion and prepare initial hybrid metal solution, wherein, iron concentration 0.3mol/L, barium ionss concentration 0.02
Mol/L, 0.02 mol/L concentration of cobalt ions of strontium ion concentration, 0.025 mol/L；With sodium hydroxide and sodium carbonate as composite precipitation
Agent, prepares composite precipitation agent solution, wherein, 2.0 mol/L of naoh concentration, concentration of sodium carbonate 0.08mol/L；Will be compound heavy
Shallow lake agent solution is added in initial hybrid metal solution with the drop speed of 10ml/min, is stirred in Deca, is stirred during Deca
Speed is 300 revs/min, and stirring reaction carries out centrifugal treating 10 minutes after 24 hours, under 9000 revs/min, washes 3 times,
After will obtain be centrifuged product i.e. precursor powder dry at 80 DEG C, using sodium chloride, potassium chloride mixture as disperse medium,
Wherein, sodium chloride is 1 with the ratio of the amount of the material of potassium chloride:1, and disperse medium quality accounts for the 50% of precursor powder quality；
Again by precursor powder and disperse medium heat treatment in high temperature furnace, 5 DEG C/min of heat treatment heating rate is warming up under 400
Insulation 30 minutes, is continuously heating to 1000 DEG C and is incubated 2 hours, is finally warming up to 1250 DEG C and is incubated 6 hours, furnace cooling；Take out
Product is cleaned with 80 DEG C of hot water afterwards, be placed in baking oven 80 DEG C and be drying to obtain final product.
The crystal structure for preparing sample is Ba1.5Sr1.5Co2Fe24O41, and crystallinity is good（Such as Fig. 1）.Using sweeping
Electron microscope observation is retouched, distribution of particles is more uniform, size is distributed in 0.5 μm mostly to 8 μm, and can see individual particle
Pattern present hexagonal plate structure（Such as Fig. 2）.It can be seen that saturation magnetization reaches from the hysteresis curve of sample
56.66emu/g, coercivity is 15.67Oe, and sample has good soft magnetic characteristic（Such as Fig. 3）.
Case study on implementation 2：
With chemical composition as Ba3Co2Fe24O41Co2Implement synthesis as a example by Z hexad ferrites：Soluble metal halogenide is selected,
Weigh according to stoichiometric proportion and prepare starting metals solution, wherein, iron concentration 0.3mol/L, barium ionss concentration 0.04
Mol/L, 0.025 mol/L of concentration of cobalt ions；With sodium hydroxide and sodium carbonate as compound precipitantses, compound precipitantses are prepared molten
Liquid, wherein, 2.0 mol/L of naoh concentration, concentration of sodium carbonate 0.08mol/L；By composite precipitation agent solution with 10ml/min
Drop speed be added in starting metals solution, stir in Deca, during Deca stir speed (S.S.) be 600 revs/min, reaction 24
Hour after, carry out centrifugal treating 10 minutes at 9000 revs/min, wash 3 times, after will obtain be centrifuged product i.e. precursor powder
Dry at 80 DEG C, using sodium chloride, potassium chloride mixture as disperse medium, wherein, sodium chloride and the material of potassium chloride
The ratio of amount is 1:1, and disperse medium quality accounts for the 50% of precursor powder quality；Again precursor powder and disperse medium are existed
Heat treatment in high temperature furnace, heat treatment heating rate are 5 DEG C/min, are warming up to 400 DEG C and are incubated 30 minutes, are continuously heating to 1000
DEG C insulation 2 hours, be finally warming up to 1250 DEG C be incubated 6 hours, furnace cooling；Product is carried out clearly with 80 DEG C of hot water after taking-up
Wash, be placed in 80 DEG C of drying to obtain final products in baking oven.
Sample is prepared for the good Ba of crystallinity3Co2Fe24O41（Such as Fig. 4）.Using sem observation,
Distribution of particles is more uniform, and size is distributed in 2 μm to 10 μm mostly, and can see that the pattern of individual particle assumes hexagonal plate
Structure（Such as Fig. 5）.It can be seen that saturation magnetization reaches 53.30emu/g from the hysteresis curve of sample, coercivity is
22.15Oe, sample assume good soft magnetic characteristic（Such as Fig. 6）.
Case study on implementation 3：
With chemical composition as Sr3Co2Fe24O41Co2Implement synthesis as a example by Z hexad ferrites：Soluble metal halogenide is selected,
Weigh according to stoichiometric proportion and prepare starting metals solution, wherein, iron concentration 0.3mol/L, strontium ion concentration 0.04
Mol/L, 0.025 mol/L of concentration of cobalt ions；With sodium hydroxide and sodium carbonate as compound precipitantses, compound precipitantses are prepared molten
Liquid, wherein, 2.0 mol/L of naoh concentration, concentration of sodium carbonate 0.08mol/L；By composite precipitation agent solution with 10ml/min
Drop speed be added in starting metals solution, stir in Deca, during Deca stir speed (S.S.) be 600 revs/min, reaction 24
Hour after, carry out centrifugal treating 10 minutes at 9000 revs/min, wash 3 times, after will obtain be centrifuged product i.e. precursor powder
Dry at 80 DEG C, using sodium chloride, potassium chloride mixture as disperse medium, wherein, sodium chloride and the material of potassium chloride
The ratio of amount is 1:1, and disperse medium quality accounts for the 50% of precursor powder quality；Again precursor powder and disperse medium are existed
Heat treatment in high temperature furnace, heat treatment heating rate are 5 DEG C/min, are warming up to 400 DEG C and are incubated 30 minutes, are continuously heating to 1000
DEG C insulation 2 hours, be finally warming up to 1250 DEG C be incubated 6 hours, furnace cooling；Product is carried out clearly with 80 DEG C of hot water after taking-up
Wash, be placed in 80 DEG C of drying to obtain final products in baking oven.
Sample is prepared for the good Sr of crystallinity3Co2Fe24O41（Such as Fig. 7）.Using sem observation,
Distribution of particles is more uniform, and size is distributed in 5 μm or so mostly, and can see that the pattern of individual particle assumes hexagonal plate knot
Structure（Such as Fig. 8）.It can be seen that saturation magnetization reaches 81.0emu/g from the hysteresis curve of sample, coercivity is
56.27Oe.（Such as Fig. 9）.
Claims (10)
1. one kind prepares high purity granular single crystallization Co2The method of Z-type ferrite powder, it is characterised in that its step is as follows：
1) according to Co2Z hexad ferrite chemical formula Ba3-xSrxCo2Fe24O41, x=0-3, weigh barium, strontium, cobalt, ferrum element solvable
Property slaine be dissolved in deionized water, obtain mixed salt solution, wherein, iron concentration be 0.5～3.0 mol/L；
2) mixture with alkali and carbonate is dissolved in deionized water, obtains compound precipitantses molten as compound precipitantses
Liquid；
3）Under agitation, composite precipitation agent solution is added step 1 with certain drop speed）In the metal salt solution；Continue
Stirring reaction is until reaction system ionic strength remains stable；
4）By step 3）Serosity after coprecipitation reaction carries out centrifugal treating, removes the centrifugation supernatant, and centrifugal deposition is through super
Sound is scattered in deionized water again through centrifugation, is cleaned repeatedly, is close to neutrality to centrifugal clear liquid；
5）Gained is centrifuged product and dries at 60～90 DEG C, and obtains presoma powder body through grinding to crush；
6）With salt-mixture as disperse medium, mix by gained presoma powder body and by mechanical ball milling with disperse medium
Even, then heat treatment is carried out, obtain synthetic product；
7）Synthetic product is ground, and adds 70～90 DEG C of hot water to clean repeatedly, remove salt medium, through 70～90 DEG C
Drying obtains target ferrite powder product.
2. the method for claim 1, it is characterised in that step 1）In, described soluble metallic salt be chlorate or
Nitrate.
3. the method for claim 1, it is characterised in that step 2）In, described alkali be sodium hydroxide, potassium hydroxide or
Ammonia；Described carbonate be sodium carbonate, potassium carbonate or ammonium carbonate, the preferred sodium hydroxide-sodium carbonate of described compound precipitantses,
Any one in potassium hydroxide-potassium carbonate and ammonia-ammonium carbonate.
4. the method for claim 1, it is characterised in that step 2）In, in composite precipitation agent solution alkali concn be 1.0～
5.0 mol/L, carbonate concentration are 0.01～0.10 mol/L.
5. the method for claim 1, it is characterised in that step 3）In, the alkali consumption in compound precipitantses is 3 times of ferrum
The 100%～150% of the amount summation of ion and 2 times of cobalt ion materials, carbonate consumption are that barium ionss are total with the amount of strontium ion material
The 100%～150% of sum.
6. the method for claim 1, it is characterised in that step 3）In, the control of the drop of composite precipitation agent solution speed 2～
Between 20 ml/ minutes, during Deca, stir speed (S.S.) is 100～600 revs/min；The stirring reaction time is 12～48 hours.
7. the method for claim 1, it is characterised in that step 4）In, centrifugal treating rotating speed be 2000～10000 turns/
Minute, the centrifugal treating time is 5～30 minutes.
8. the method for claim 1, it is characterised in that step 6）In, described disperse medium adopts sodium chloride, chlorination
Any two kinds or its thing mixed above in potassium, sodium sulfate and potassium sulfate, in mixture, the mol ratio of each material is 1:1；Dispersion is situated between
The consumption of matter for precursor weight 30% ~ 400%.
9. the method for claim 1, it is characterised in that step 6）In, in mechanical ball milling, ratio of grinding media to material is 10:1～5:1,
Ball milling speed is 100～400 revs/min, and Ball-milling Time is 1～8 hour.
10. the method for claim 1, it is characterised in that step 6）In, the heating rate of heat treatment is 2～10 DEG C/
Minute, heat treatment process is at 400 DEG C to be incubated 30 minutes～2 hours, is continuously heating to be incubated 1～4 hour at 1000 DEG C,
It is warming up at 1150～1300 DEG C again and is incubated 4～12 hours.
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Cited By (6)
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| CN110136907A (en) * | 2019-04-26 | 2019-08-16 | 南京睿磐内尔环保复合新材料有限公司 | A kind of method of ultrasonic wave added Co deposited synthesis complex ferrite |
| CN110182853A (en) * | 2019-05-10 | 2019-08-30 | 江辉 | A kind of preparation method of Co-Ti codope hexad ferrite nano-powder |
| CN112679205A (en) * | 2020-12-29 | 2021-04-20 | 横店集团东磁股份有限公司 | Z-type ferrite and preparation method thereof |
| CN112851326A (en) * | 2021-01-29 | 2021-05-28 | 兰州大学 | Co2Z-type ferrite material and preparation method thereof |
| CN113744991A (en) * | 2021-09-17 | 2021-12-03 | 横店集团东磁股份有限公司 | Co2Z-type ferrite material and preparation method and application thereof |
| CN113968730A (en) * | 2021-11-11 | 2022-01-25 | 横店集团东磁股份有限公司 | Z-type ferrite composite 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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| CN110136907A (en) * | 2019-04-26 | 2019-08-16 | 南京睿磐内尔环保复合新材料有限公司 | A kind of method of ultrasonic wave added Co deposited synthesis complex ferrite |
| CN110182853A (en) * | 2019-05-10 | 2019-08-30 | 江辉 | A kind of preparation method of Co-Ti codope hexad ferrite nano-powder |
| CN112679205A (en) * | 2020-12-29 | 2021-04-20 | 横店集团东磁股份有限公司 | Z-type ferrite and preparation method thereof |
| CN112679205B (en) * | 2020-12-29 | 2022-02-22 | 横店集团东磁股份有限公司 | Z-type ferrite and preparation method thereof |
| CN112851326A (en) * | 2021-01-29 | 2021-05-28 | 兰州大学 | Co2Z-type ferrite material and preparation method thereof |
| CN113744991A (en) * | 2021-09-17 | 2021-12-03 | 横店集团东磁股份有限公司 | Co2Z-type ferrite material and preparation method and application thereof |
| CN113968730A (en) * | 2021-11-11 | 2022-01-25 | 横店集团东磁股份有限公司 | Z-type ferrite composite material and preparation method and application thereof |
| CN113968730B (en) * | 2021-11-11 | 2023-01-10 | 横店集团东磁股份有限公司 | Z-type ferrite composite material and preparation method and application thereof |
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Application publication date: 20170315 |