CN107792889A - A kind of strontium cobalt W type hexad ferrite materials and preparation method thereof - Google Patents
A kind of strontium cobalt W type hexad ferrite materials and preparation method thereof Download PDFInfo
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- CN107792889A CN107792889A CN201711065560.5A CN201711065560A CN107792889A CN 107792889 A CN107792889 A CN 107792889A CN 201711065560 A CN201711065560 A CN 201711065560A CN 107792889 A CN107792889 A CN 107792889A
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/006—Compounds containing, besides cobalt, two or more other elements, with the exception of oxygen or hydrogen
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
Abstract
The invention discloses a kind of strontium cobalt W type hexad ferrite materials and preparation method thereof, be using strontium salt, cobalt salt and molysite as raw material, with NaOH reactants, after being well mixed, after hydro-thermal method, through filtering, clean, calcine made from molecular formula be SrxCoyFezO27Strontium cobalt W type hexad ferrite materials, the preparation method technique is simple, and the powder finally prepared is easily dispersed, and is not required to ball milling again, avoids impurity and fault of construction caused by ball milling etc. post-processes；Microscopic appearance development is complete, regular hexagonal plate is presented, material granule purity is higher, good dispersion, even size distribution, also has the higher intensity of magnetization and low-coercivity.
Description
Technical field
The present invention relates to ferrite magnetic material preparing technical field, specifically a kind of strontium cobalt W type hexad ferrite materials
And preparation method thereof.
Background technology
At present, ferrite can be divided into spinel type ferrite, garnet type ferrite and magneto-plumbite type ferrite.Magneto-plumbite type
Type ferrite wherein hexgonal screw is to belong to hexaplanar, including M, X, Y, U, Z, W-type ferrite.W type hexagonal crystalline forms
Ferrite is applied to magnetic recording and electronic component due to its high saturation rate, high-coercive force, good chemical stability
Deng field.The preparation technology of Ferrite Material is broadly divided into the major class of dry and wet two, and dry method main representative is solid-phase ball milling method,
Solid phase method is simple to operate, is easy to large-scale industrial production, but reactant activity is not high, is easy to reunite.Wet method includes co-precipitation again
Method, sol-gal process, hydro-thermal method and solvent-thermal method etc..Wet method, which prepares ferrite, can then make up the deficiency of dry process, and use is wet
The advantages that particulate prepared by method has purity height, even particle size distribution, and activity is good.Also just so, wet method preparation process is near
The development of abundance has been obtained over year.Wherein hydro-thermal method synthesis hexad ferrite is used by increasing people, and application prospect
It is very wide.Yet with the complexity of strontium cobalt hexad ferrite structure, current ripe hydro-thermal method successfully prepares strontium cobalt hexagonal
Ferrite is also seldom, and poor performance.
The content of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to and provide a kind of strontium cobalt W types hexad ferrite material and
Its preparation method, the preparation method technique is simple, and the powder finally prepared is easily dispersed, and is not required to ball milling again, avoids because of ball
Impurity and fault of construction caused by the post processing such as mill；Microscopic appearance development is complete, regular hexagonal plate is presented, material granule is pure
Higher, good dispersion is spent, even size distribution, also there is the higher intensity of magnetization and low-coercivity.
Realizing the technical scheme of the object of the invention is：
A kind of strontium cobalt W type hexad ferrite materials, it is using strontium salt, cobalt salt and molysite as raw material, with NaOH reactants, is well mixed
Afterwards, after using hydro-thermal method, through filtering, clean, calcine made from molecular formula be SrxCoyFezO27Strontium cobalt W type hexad ferrite materials
Material.
The mol ratio of described strontium salt, cobalt salt and molysite is x：y：z=1：1.5-2：15-16.
Described NaOH and the mol ratio of metal ion are 3-3.5：1.
Described strontium salt, cobalt salt, molysite are nitrate or villaumite.
The strontium salt is Sr (NO3 ) 2Or SrCl26H2O；Described cobalt salt is Co (NO3 ) 2 .6 H2O or
CoCl2 ；Described molysite is Fe (NO3 ) 3 . 9 H2O or FeCl3.
A kind of preparation method of strontium cobalt W type hexad ferrite materials, specifically comprises the following steps：
1）It is 1 by metal ion mol ratio：1.5-2：15-16 weighs strontium salt, cobalt salt and molysite successively, is configured to distilled water
Even mixing salt solution, then in the ratio that NaOH and total metal ion mol ratio are 3.0-3.5 weigh NaOH to be configured to NaOH molten
Liquid, add in mixing salt solution, be well mixed, hydro-thermal presoma is made；
2）By step 1）Obtained hydro-thermal presoma is fitted into hydrothermal reaction kettle, ultrasonic 15-20min, after ultrasonic disperse is uniform, enters
Water-filling thermal response, is naturally cooling to room temperature, and the presoma of strontium cobalt W type hexad ferrite materials is made；
3）By step 2）The presoma of obtained strontium cobalt W type hexad ferrite materials takes out from reactor, is filtered, clearly
Wash, the PH of the presoma of strontium cobalt W type hexad ferrite materials is adjusted to neutrality, be then dried to obtain strontium cobalt W type hexgon iron oxygen
Body material xeraphium；
4）By step 3）Obtained strontium cobalt W type hexad ferrite material xeraphiums, are placed in agate mortar and add alcohol, fully grind
Grinds, then calcined in Muffle furnace, final strontium cobalt W type hexad ferrite materials are made after cooling.
Step 2）In, described hydro-thermal reaction, temperature is 180 ~ 200 DEG C, and the reaction time is 5 ~ 40h.
Step 4）In, described calcining, it is with 2 DEG C/min programming rate, is warming up to 1190 ~ 1280 DEG C of calcining 1-
4h。
Beneficial effect：A kind of strontium cobalt W type hexad ferrite materials provided by the invention and preparation method thereof, the material pass through
Hydro-thermal reaction, with the rise of hydrothermal temperature, the activity of water can increase, and improve reaction speed, can effectively reduce miscellaneous
The absorption of matter so that the material in hydrothermal reaction kettle can sufficiently react.Powder can be made to be uniformly dispersed, polymerization is few, prepares
Go out the higher W-type ferrite of purity, so as to improve its saturation magnetization.Material after in water heating kettle was carried out
Filter, cleaning, dry, obtain high-coercive force hexagonal plate strontium Conjugate ferrite particle.The hexagonal plate strontium synthesized using this method
Not only purity is higher for Conjugate ferrite particle, good dispersion, even size distribution, also has the higher intensity of magnetization and low coercive
Power, the sample have preferable application prospect in the motor of electrical equipment, loudspeaker, high frequency magnetic recording.
Brief description of the drawings
Fig. 1 is a kind of preparation method process chart of strontium cobalt W type hexad ferrite materials of the present invention；
Fig. 2 is the x ray diffraction collection of illustrative plates of strontium cobalt W type hexad ferrite materials prepared by embodiment 4（XRD）；
Fig. 3 is the scanning electron microscope (SEM) photograph of strontium cobalt W type hexad ferrite materials prepared by embodiment 4（SEM）；
Fig. 4 is the hysteresis curve figure for the strontium cobalt W type hexad ferrite materials that embodiment 1,2,3,4 is prepared（M-H）；
Find out that sample prepared by the present invention is strontium cobalt W type hexad ferrites from Fig. 2 XRD；It is from figure 3, it can be seen that of the invention
The ferrite particle diameter of preparation is 5 microns, is evenly distributed；As can be seen from Figure 4, the ferrite saturation magnetization that prepared by the present invention is most
Height is about 78 ~ 80 emu/g, has higher magnetic, and coercivity is about 200 ~ 700Oe, is prepared well below other preparation methods
Strontium Conjugate ferrite.
Embodiment
The present invention is further elaborated with reference to embodiment, but is not limitation of the invention.
Embodiment 1：
A kind of preparation method of strontium cobalt W type hexad ferrite materials, specifically comprises the following steps：
1）Mol ratio is weighed successively as 1：1.5：15 Sr (NO3 ) 2、Co ( NO3 ) 2 .6 H2O、Fe ( NO3 ) 3 . 9
H2O, mixing salt solution is configured to distilled water, stirs half an hour at room temperature on magnetic stirring apparatus.Stirred placing magnetic force
Mix device to go forward, rotating speed is set to zero, splashed to prevent solution.According to metal ion ratio, according to NaOH：Metal ion mol ratio
About 3, it is sufficiently stirred dissolving after weighing NaOH.Using NaOH as precipitating reagent, it is slowly dropped into rubber head dropper in mixing salt solution,
During this, magnetic stirring apparatus works on and obtains hydro-thermal presoma calmly.
2）By step 1）Obtained hydro-thermal presoma is fitted into the reactor polytetrafluoroethylliner liner that capacity is 50ml,
It is cleaned by ultrasonic ultrasonic 15min in instrument, makes presoma more dispersed, dress kettle, envelope kettle is anti-at 180 DEG C in air dry oven
5h is answered, is naturally cooling to room temperature, the presoma of strontium cobalt W type hexad ferrite materials is made.
3）By step 2）The presoma of obtained strontium cobalt W type hexad ferrite materials, takes out from water heating kettle, by multiple
Filtering, is continuously added into deionized water and alcohol is rinsed, the foreign ion in reactant is flushed out, dripped when from filter paper therebetween
When the solution PH to get off is close to 7, stop filtering, then remaining product is placed on inside baking oven and dried, obtains strontium
Cobalt W type hexad ferrite material xeraphiums.
4）By step 3）Obtained strontium cobalt W type hexad ferrite material xeraphiums, which are placed in agate mortar, adds alcohol, fills
Divide and pulverize, being warming up to 1190 DEG C in Muffle furnace with 2 °/min is calcined, soaking time 1h, is made after cooling
Final strontium cobalt W type hexad ferrite materials.
Embodiment 2：
A kind of preparation method of strontium cobalt W type hexad ferrite materials, specifically comprises the following steps：
1）Mol ratio is weighed successively as 1：1.75：15.5 SrCl2·6H2O、CoCl2、FeCl3, it is configured to mix with distilled water
Salting liquid, stir half an hour at room temperature on magnetic stirring apparatus.Gone forward placing magnetic stirring apparatus, rotating speed is adjusted to
Zero, splashed to prevent solution.According to metal ion ratio, according to NaOH：Metal ion mol ratio is about 3.2, is filled after weighing NaOH
Divide stirring and dissolving.Using NaOH as precipitating reagent, it is slowly dropped into rubber head dropper in mixing salt solution, during this, magnetic agitation
Device works on and obtains hydro-thermal presoma calmly.
2）By step 1）Obtained hydro-thermal presoma is fitted into the reactor polytetrafluoroethylliner liner that capacity is 50ml,
It is cleaned by ultrasonic ultrasonic 15min in instrument, makes presoma more dispersed, dress kettle, envelope kettle is anti-at 180 DEG C in air dry oven
10h is answered, is naturally cooling to room temperature, the presoma of strontium cobalt W type hexad ferrite materials is made.
3）By step 2）The presoma of obtained strontium cobalt W type hexad ferrite materials, takes out from water heating kettle, by multiple
Filtering, is continuously added into deionized water and alcohol is rinsed, the foreign ion in reactant is flushed out, dripped when from filter paper therebetween
When the solution PH to get off is close to 7, stop filtering, then remaining product is placed on inside baking oven and dried, obtains strontium
Cobalt W type hexad ferrite material xeraphiums.
4）By step 3）Obtained strontium cobalt W type hexad ferrite material xeraphiums, which are placed in agate mortar, adds alcohol, fills
Divide and pulverize, being warming up to 1250 DEG C in Muffle furnace with 2 °/min is calcined, soaking time 2h, is made after cooling
Final strontium cobalt W type hexad ferrite materials.
Embodiment 3：
A kind of preparation method of strontium cobalt W type hexad ferrite materials, specifically comprises the following steps：
1）Mol ratio is weighed successively as 1：2：16 Sr (NO3 ) 2Or SrCl2·6H2O, Co (NO3 ) 2 .6 H2O or
CoCl2, Fe (NO3 ) 3 . 9 H2O or FeCl3, stir half an hour at room temperature on magnetic stirring apparatus.Placing magnetic force
Agitator is gone forward, and rotating speed is set to zero, and is splashed to prevent solution.According to metal ion ratio, according to NaOH：Metal ion mole
Than being about 3.5, dissolving is sufficiently stirred after weighing NaOH.Using NaOH as precipitating reagent, it is molten to be slowly dropped into salt-mixture with rubber head dropper
In liquid, during this, magnetic stirring apparatus works on and obtains hydro-thermal presoma calmly.
2）By step 1）Obtained hydro-thermal presoma is fitted into the reactor polytetrafluoroethylliner liner that capacity is 50ml,
It is cleaned by ultrasonic ultrasonic 15min in instrument, makes presoma more dispersed, dress kettle, envelope kettle is anti-at 200 DEG C in air dry oven
20h is answered, is naturally cooling to room temperature, the presoma of strontium cobalt W type hexad ferrite materials is made.
3）By step 2）The presoma of obtained strontium cobalt W type hexad ferrite materials, takes out from water heating kettle, by multiple
Filtering, is continuously added into deionized water and alcohol is rinsed, the foreign ion in reactant is flushed out, dripped when from filter paper therebetween
When the solution PH to get off is close to 7, stop filtering, then remaining product is placed on inside baking oven and dried, obtains strontium
Cobalt W type hexad ferrite material xeraphiums.
4）By step 3）Obtained strontium cobalt W type hexad ferrite material xeraphiums, which are placed in agate mortar, adds alcohol, fills
Divide and pulverize, being warming up to 1280 DEG C in Muffle furnace with 2 °/min is calcined, soaking time 3h, is made after cooling
Final strontium cobalt W type hexad ferrite materials.
Embodiment 4：
A kind of preparation method of strontium cobalt W type hexad ferrite materials, specifically comprises the following steps：
1）Mol ratio is weighed successively as 1：2：16 Sr (NO3 ) 2, Co (NO3 ) 2 .6 H2O, Fe (NO3 ) 3 . 9
H2O, mixing salt solution is configured to distilled water, stirs half an hour at room temperature on magnetic stirring apparatus.Stirred placing magnetic force
Mix device to go forward, rotating speed is set to zero, splashed to prevent solution.According to metal ion ratio, according to NaOH：Metal ion mol ratio
About 3.5, it is sufficiently stirred dissolving after weighing NaOH.Using NaOH as precipitating reagent, mixing salt solution is slowly dropped into rubber head dropper
In, during this, magnetic stirring apparatus works on and obtains hydro-thermal presoma calmly.
2）By step 1）Obtained hydro-thermal presoma is fitted into the reactor polytetrafluoroethylliner liner that capacity is 50ml,
It is cleaned by ultrasonic ultrasonic 15min in instrument, makes presoma more dispersed, dress kettle, envelope kettle is anti-at 200 DEG C in air dry oven
40h is answered, is naturally cooling to room temperature, the presoma of strontium cobalt W type hexad ferrite materials is made.
3）By step 2）The presoma of obtained strontium cobalt W type hexad ferrite materials, takes out from water heating kettle, by multiple
Filtering, is continuously added into deionized water and alcohol is rinsed, the foreign ion in reactant is flushed out, dripped when from filter paper therebetween
When the solution PH to get off is close to 7, stop filtering, then remaining product is placed on inside baking oven and dried, obtains strontium
Cobalt W type hexad ferrite material xeraphiums.
4）By step 3）Obtained strontium cobalt W type hexad ferrite material xeraphiums, which are placed in agate mortar, adds alcohol, fills
Divide and pulverize, being warming up to 1280 DEG C in Muffle furnace with 2 °/min is calcined, soaking time 4h, is made after cooling
Final strontium cobalt W type hexad ferrite materials.
Claims (10)
- A kind of 1. strontium cobalt W type hexad ferrite materials, it is characterised in that be using strontium salt, cobalt salt and molysite as raw material, it is anti-with NaOH Agent is answered, after being well mixed, uses molecular formula made from hydro-thermal method as SrxCoyFezO27Strontium cobalt W type hexad ferrite materials.
- 2. a kind of strontium cobalt W type hexad ferrite materials according to claim 1, it is characterised in that described strontium salt, cobalt salt Mol ratio with molysite is x：y：z=1：1.5-2：15-16.
- 3. a kind of strontium cobalt W type hexad ferrite materials according to claim 1, it is characterised in that described NaOH and gold The mol ratio for belonging to ion is 3-3.5：1.
- 4. a kind of strontium cobalt W type hexad ferrite materials according to claim 1, it is characterised in that described strontium salt, cobalt Salt, molysite are nitrate or villaumite.
- 5. a kind of strontium cobalt W type hexad ferrite materials according to claim 4, it is characterised in that described strontium salt is Sr ( NO3 ) 2Or SrCl2·6H2O。
- 6. a kind of strontium cobalt W type hexad ferrite materials according to claim 4, it is characterised in that described cobalt salt is Co ( NO3 ) 2 .6 H2O or CoCl2。
- 7. a kind of strontium cobalt W type hexad ferrite materials according to claim 4, it is characterised in that described molysite is Fe ( NO3 ) 3 . 9 H2O or FeCl3。
- 8. a kind of preparation method of strontium cobalt W type hexad ferrite materials, it is characterised in that specifically comprise the following steps：1）It is 1 by metal ion mol ratio：1.5-2：15-16 weighs strontium salt, cobalt salt and molysite successively, is configured to distilled water Even mixing salt solution, then in the ratio that NaOH and total metal ion mol ratio are 3.0-3.5 weigh NaOH to be configured to NaOH molten Liquid, add in mixing salt solution, be well mixed, hydro-thermal presoma is made；2）By step 1）Obtained hydro-thermal presoma is fitted into hydrothermal reaction kettle, ultrasonic 15-20min, after ultrasonic disperse is uniform, enters Water-filling thermal response, is naturally cooling to room temperature, and the presoma of strontium cobalt W type hexad ferrite materials is made；3）By step 2）The presoma of obtained strontium cobalt W type hexad ferrite materials takes out from reactor, is filtered, clearly Wash, the PH of the presoma of strontium cobalt W type hexad ferrite materials is adjusted to neutrality, be then dried to obtain strontium cobalt W type hexgon iron oxygen Body material xeraphium；4）By step 3）Obtained strontium cobalt W type hexad ferrite material xeraphiums, are placed in agate mortar and add alcohol, fully grind Grinds, then calcined in Muffle furnace, final strontium cobalt W type hexad ferrite materials are made after cooling.
- A kind of 9. preparation method of strontium cobalt W type hexad ferrite materials according to claim 8, it is characterised in that step 2）In, described hydro-thermal reaction, temperature is 180 ~ 200 DEG C, and the reaction time is 5 ~ 40h.
- A kind of 10. preparation method of strontium cobalt W type hexad ferrite materials according to claim 8, it is characterised in that step 4）In, described calcining, it is with 2 DEG C/min programming rate, is warming up to 1190 ~ 1280 DEG C of calcining 1-4h.
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| CN110862595A (en) * | 2019-12-12 | 2020-03-06 | 黄春美 | Super-hydrophobic modified hydrogenated nitrile rubber magnetic composite material and preparation method thereof |
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Application publication date: 20180313 |