CN108409316A - A kind of preparation method of low magnetic loss magnetic material - Google Patents
A kind of preparation method of low magnetic loss magnetic material Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of low magnetic loss magnetic material, belong to magnetic material preparing technical field.When the present invention prepares manganese compound, by multi-step impurity removal process, reduce the content of iron, sintering temperature is raised to higher temperature by the present invention first when being sintered, when sintering temperature then being dropped to lower temperature, heat preservation a period of time, it can make the magnetic material that sintering obtains that there is evenly tiny particle and higher density, wherein iron oxide is uniformly distributed in magnetic material, highdensity magnetic induction curve can be generated by working under magnetic material for transformer, improve the saturation flux density of magnetic material, slurry is sintered using organic solvent polyvinyl alcohol as binding material, compared to silica, titanium dioxide isogel binding material, the Curie temperature of magnetic material can be made to become higher, increase saturation flux density, so that low magnetic loss magnetic material has high saturation magnetic flux density, it has a extensive future.
Description
Technical field
The invention discloses a kind of preparation methods of low magnetic loss magnetic material, belong to magnetic material preparing technical field.
Background technology
Magnetic material, usually said magnetic material refer to ferromagnetic substance, are functions ancient and that purposes is very extensive
Material.Modem magnetic materials have been widely used among our life, such as permanent-magnet material is used as motor, are applied to become
Core material in depressor, as the magneto-optic disk that memory uses, computer magnetic recording floppy disk etc..After magnetic material is by magnetization
The difficulty or ease of degaussing can be divided into soft magnetic material and retentive material.It is easy to remove magnetic substance after magnetization soft magnetic material,
It is not easy the substance of degaussing retentive material.Soft magnetic material remanent magnetism in general is smaller, and retentive material remanent magnetism is larger.
The development experience of magnetic material from inorganic to organic, solid-state to liquid, macroscopic view to be situated between see, electronics magnetic order to core
Magnetic order ferromagnetic material, single type to magnetic property and overall characteristic compound, and that show excellent.Magnetic material is due to dividing
Class standard and emphasis difference, there is different classification.General magnetic material can be divided by application type classification：Permanent magnetism material
Material, soft magnetic materials etc..Magnetic material be primarily referred to as by transition elements iron, cobalt, nickel and its alloy etc. form can directly or
It practices midwifery the substance of magnetisation.From application function, magnetic material is divided into：Soft magnetic materials, permanent-magnet material, magnetic recording-square magnetic material
The types such as material, gyromagnetic material.Magnetic material is the important foundation functional material of electronics industry, is widely used in computer, electronics
The daily necessities such as the industrial circles such as device, communication, automobile and aerospace and household electrical appliance, toy for children, with the world
The demand of economic and science and technology fast development, magnetic material will be unprecedented wide.Magnetic material is in electronics, computer, information
The tradition such as communication, medical treatment, aerospace, automobile, wind-powered electricity generation, environmental protection and energy saving and emerging field all play an important role.It is magnetic
Material, which has become, promotes hi-tech development and the irreplaceable material of modern economy progress.
As the development of electronic communication is to ensure information by being electromagnetically shielded protection information from full spectrum of threats and interference
The important means of safety.In actual electromagnetic shielding application, effective shield effectiveness standard is 20dB.Due to all kinds of electronic communication devices
The integrated and facilitation of part, the demand to lightweight, thin layer, High Performance Shielding are also more and more urgent.Magnetic material at present
Power attenuation is big when as magnetic core, and when magnetic material is used as field transformer, magnetic permeability is relatively high, but saturation flux density is very
It is low, it is only applicable to high inductance reduced-current requirement occasion.
Therefore, invent a kind of magnetic material that magnetic loss is low has positive effect to magnetic material preparing technical field.
Invention content
Present invention mainly solves the technical issues of, for current magnetic material be used as magnetic core when power attenuation it is big, magnetic material
When material is used as field transformer, magnetic permeability is relatively high, but saturation flux density is very low, is only applicable to high inductance reduced-current and wants
The defect for seeking occasion provides a kind of preparation method of low magnetic loss magnetic material.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of preparation method of low magnetic loss magnetic material, it is characterised in that specifically preparation process is：
（1）It takes 100~110g pyrolusite stones to be placed in pulverizer to crush, sieving obtains pyrolusite powder, and pyrolusite powder is placed in instead
It answers in kettle, 40~50g iron powders, 200~300mL concentrated sulfuric acid solutions and 20~30g orange peels is added to reaction kettle, is stirred
Afterwards, reaction kettle is moved into water-bath, heat temperature raising, insulation reaction, filtering removal filter residue obtains leachate；
（2）Into above-mentioned leachate be added 70~80g manganese dioxide, heat temperature raising, reaction, obtain Oxidation Leaching liquid, continue to
30~40g manganese carbonates are added in Oxidation Leaching liquid, stirring filters Oxidation Leaching liquid until bubble generation, collects filtrate,
Filtrate is transferred in beaker, ammonium hydroxide is added into beaker, adjusts pH, is separated by filtration to obtain deep iron removal after stirring 5~10min
Liquid；
（3）100~120mL ammonium sulfide solutions are added into deep iron removal liquid, heat temperature raising starts magnetic stirring apparatus, with 200~
After the rotating speed of 250r/min is stirred to react, standing, filtering removal flocculate obtains clarified solution, continuously add 8 into clarified solution~
10g ammonium fluorides, heat temperature raising are stirred to react, the manganese sulfate solution after being purified；
（4）The above-mentioned manganese sulfate solutions of 300~350mL are placed in beaker, 70~80mL absolute ethyl alcohols are added to beaker, then use ammonia
Water adjusts pH value of solution in beaker, and beaker is moved into water-bath, is heated to 75~80 DEG C, with turning for 700~800r/min
Speed stirs and is passed through air into beaker after insulated and stirred reaction with air blower and pours into solution in beaker in evaporating dish, heats
Heating, evaporation, purification obtain manganese compound；
（5）Iron oxide, zinc oxide, above-mentioned manganese compound are mixed, mixture to be ground is obtained, mixture to be ground and polyvinyl alcohol is molten
Liquid is mixed to get suspension, and suspension is put into ball mill, then ball milling pearl is added into ball mill by certain ball material mass ratio,
Ball milling obtains magnetic core slurry；
（6）Magnetic core slurry is poured into cylindrical die, mold is put into after suppressing 5~8min in forcing press, mold is put into
It is sintered in resistance furnace, is demoulded after cooled to room temperature and obtain low magnetic loss magnetic material.
Step（1）The be sieved specification is 100 mesh, and the mass fraction of concentrated sulfuric acid solution is 45%, is stirred the time
For 20~30min, temperature is 50~55 DEG C after heat temperature raising, and the insulation reaction time is 2~3h.
Step（2）Temperature is 80~90 DEG C after the heat temperature raising, and the reaction time is 2~3h, ammonium hydroxide quality point
Number is 25%, and it is 6.5~7.0 to adjust pH.
Step（3）The mass fraction of the ammonium sulfide solution is 20%, is heated to 70~80 DEG C, when being stirred to react
Between be 1~2h, time of repose be 2~3 days, after heat temperature raising temperature be 80~90 DEG C, be stirred to react the time be 45~50min.
Step（4）It is 6.5~6.8 that the ammonium hydroxide, which adjusts pH value of solution in beaker, and temperature is 75~80 DEG C after heat temperature raising,
It is 20~30L/min that air blower, which is passed through air speed into beaker, and the insulated and stirred reaction time is 40~45min, and evaporating dish adds
Temperature is 120~130 DEG C after heat heating, and evaporation time is 1~2h.
Step（5）The iron oxide, zinc oxide, manganese compound mixing quality ratio are 5 ︰, 1 ︰ 3, mixture and polyethylene to be ground
Alcoholic solution is 1 ︰ 3 in mass ratio, and poly-vinyl alcohol solution mass fraction is 25%, and ball material mass ratio is 20:1, ball milling bead diameter is
0.1~0.3mm, Ball-milling Time are 15~20h.
Step（6）The pressing pressure is 6~8MPa, and sintering process is：The rate of 2~3 DEG C/min is warming up to 1050
~1100 DEG C, 2~3h of heat preservation sintering, after continuation rises to 1200~1250 DEG C with same heating rate, it is naturally cooling to 1050
~1100 DEG C, 1~2h of heat preservation sintering.
The beneficial effects of the invention are as follows：
（1）The manganese dioxide of present invention orange peel, iron powder in sulfuric acid solution in reducing leached pyrolusite ore obtains containing manganese ion
Leachate, manganese dioxide is added into leachate, in a heated condition the low valence metal ions such as iron protoxide ion, then plus
Enter manganese carbonate hydrolytic precipitation, be filtered to remove iron ion in leachate, with ammonium sulfide solution precipitate remove leachate in heavy metal from
Son, again with ammonium fluoride be added leachate, be settled out calcium and magnesium ion, the manganese sulfate solution of purification be obtained by filtration, manganese sulfate solution is straight
It connects after being passed through air oxidation in a heated condition, evaporation purification obtains manganese compound, by iron oxide, manganese compound, zinc oxide and poly- second
Enolate solution is mixed to get suspension, and low magnetic loss magnetic material, system of the present invention are obtained through ball milling, die-filling compression moulding, sintering
When standby manganese compound, by multi-step impurity removal process, the content of iron is reduced, core loss, prepared magnetic material tool can be reduced
There are narrow magnetic induction curve, dc resistivity very high, it is possible to reduce the generation of vortex, to reduce core loss and improve magnetic
Property material saturation flux density；
（2）Sintering temperature is raised to higher temperature by the present invention first when being sintered, when sintering temperature then being dropped to lower temperature,
Heat preservation a period of time, in this stage, crystal grain is not grown significantly, by controlling the variation of temperature, is inhibiting crystal boundary migration
While leading to grain growth, grain boundary decision is kept to be in active state, the Growing Process of Crystal Particles in sintering later stage is avoided, in crystal grain
Non-growing period completes sintering, so that sintering is continued and realizes densification, the magnetic material that sintering obtains can be made to have
Evenly tiny particle and higher density, wherein iron oxide are uniformly distributed in magnetic material, by magnetic material for becoming
Highdensity magnetic induction curve can be generated by working under depressor, improve the saturation flux density of magnetic material, sintering slurry is with organic
Solvent polyvinyl alcohol is binding material can make Curie's temperature of magnetic material compared to silica, titanium dioxide isogel binding material
Degree becomes higher, increases saturation flux density, so that low magnetic loss magnetic material has high saturation magnetic flux density, before
Scape is wide.
Specific implementation mode
It takes 100~110g pyrolusite stones to be placed in pulverizer to crush, sieves with 100 mesh sieve to obtain pyrolusite powder, by pyrolusite powder
It is placed in reaction kettle, to the concentrated sulfuric acid solution and 20 that 40~50g iron powders are added in reaction kettle, 200~300mL mass fractions are 45%
After being stirred 20~30min, reaction kettle is moved into water-bath for~30g orange peels, is heated to 50~55 DEG C, heat preservation
2~3h is reacted, filtering removal filter residue obtains leachate；70~80g manganese dioxide, heat temperature raising are added into above-mentioned leachate
To 80~90 DEG C, 2~3h is reacted, Oxidation Leaching liquid is obtained, continues that 30~40g manganese carbonates are added into Oxidation Leaching liquid, stirring
Until bubble generates, Oxidation Leaching liquid is filtered, filtrate is collected, filtrate is transferred in beaker, matter is added into beaker
The ammonium hydroxide that score is 25% is measured, it is 6.5~7.0 to adjust pH, is separated by filtration to obtain deep iron removal liquid after stirring 5~10min；Xiang Shen
Degree is heated to 70~80 DEG C, starts magnetic force except the ammonium sulfide solution that 100~120mL mass fractions are 20% is added in iron liquid
Blender after being stirred to react 1~2h with the rotating speed of 200~250r/min, stands 2~3 days, and filtering removal flocculate is clarified
Liquid continuously adds 8~10g ammonium fluorides into clarified solution, is heated to 80~90 DEG C, is stirred to react 45~50min, obtains net
Manganese sulfate solution after change；The above-mentioned manganese sulfate solutions of 300~350mL are placed in beaker, it is anhydrous that 70~80mL is added to beaker
Ethyl alcohol, then adjust pH value of solution in beaker with ammonium hydroxide and beaker is moved into water-bath, is heated to 75~80 to 6.5~6.8
DEG C, it is stirred with the rotating speed of 700~800r/min and air is passed through with the rate of 20~30L/min into beaker with air blower, protected
After temperature is stirred to react 40~45min, solution in beaker is poured into evaporating dish, is heated to 120~130 DEG C, evaporation 1~
2h, purification obtain manganese compound；It is that 5 ︰, 1 ︰ 3 are mixed in mass ratio by iron oxide, zinc oxide, above-mentioned manganese compound, obtains waiting for mill mixing
The poly-vinyl alcohol solution that mixture to be ground and mass fraction are 25% is that 1 ︰ 3 is mixed to get suspension in mass ratio, will hanged by material
Supernatant liquid is put into ball mill, then it is 20 to press ball material mass ratio:1 the ball milling pearl that grain size is 0.1~0.3mm is added into ball mill,
15~20h of ball milling obtains magnetic core slurry；Magnetic core slurry is poured into cylindrical die, mold is put into forcing press with 6~
After the pressure of 8MPa suppresses 5~8min, mold is put into resistance furnace, 1050~1100 are warming up to the rate of 2~3 DEG C/min
DEG C, 2~3h of heat preservation sintering is naturally cooling to 1050~1100 after continuation rises to 1200~1250 DEG C with same heating rate
DEG C, 1~2h of heat preservation sintering, after cooled to room temperature demoulding obtain low magnetic loss magnetic material.
Example 1
It takes 100g pyrolusite stones to be placed in pulverizer to crush, sieves with 100 mesh sieve to obtain pyrolusite powder, pyrolusite powder is placed in reaction kettle
In, to the concentrated sulfuric acid solution and 20g orange peels that 40g iron powders are added in reaction kettle, 200mL mass fractions are 45%, it is stirred
After 20min, reaction kettle is moved into water-bath, is heated to 50 DEG C, insulation reaction 2h, filtering removal filter residue is leached
Liquid；70g manganese dioxide is added into above-mentioned leachate, is heated to 80 DEG C, reacts 2h, obtains Oxidation Leaching liquid, continue to
30g manganese carbonates are added in Oxidation Leaching liquid, stirring filters Oxidation Leaching liquid until bubble generation, collects filtrate, will filter
Liquid is transferred in beaker, and the ammonium hydroxide that mass fraction is 25% is added into beaker, and it is 6.5 to adjust pH, is separated by filtration after stirring 5min
Obtain deep iron removal liquid；The ammonium sulfide solution that 100mL mass fractions are 20% is added into deep iron removal liquid, is heated to 70
DEG C, start magnetic stirring apparatus, after being stirred to react 1h with the rotating speed of 200r/min, stand 2 days, filtering removal flocculate is clarified
Liquid continuously adds 8g ammonium fluorides into clarified solution, is heated to 80 DEG C, is stirred to react 45min, the manganese sulfate after being purified
Solution；The above-mentioned manganese sulfate solutions of 300mL are placed in beaker, 70mL absolute ethyl alcohols are added to beaker, then beaker is adjusted with ammonium hydroxide
Beaker is moved into water-bath to 6.5, is heated to 75 DEG C, is stirred with the rotating speed of 700r/min and use air blast by middle pH value of solution
Machine is passed through air with the rate of 20L/min into beaker and solution in beaker is poured into evaporating dish after insulated and stirred reacts 40min
In, 120 DEG C are heated to, 1h is evaporated, purification obtains manganese compound；It is in mass ratio by iron oxide, zinc oxide, above-mentioned manganese compound
5 ︰, 1 ︰ 3 mixing, obtains mixture to be ground, is in mass ratio by the poly-vinyl alcohol solution that mixture to be ground is 25% with mass fraction
1 ︰ 3 is mixed to get suspension, and suspension is put into ball mill, then it is 20 to press ball material mass ratio:1 grain size is added into ball mill
For the ball milling pearl of 0.1mm, ball milling 15h obtains magnetic core slurry；Magnetic core slurry is poured into cylindrical die, mold is put into pressure
After suppressing 5min in power machine with the pressure of 6MPa, mold is put into resistance furnace, 1050 DEG C are warming up to the rate of 2 DEG C/min,
Heat preservation sintering 2h after continuation rises to 1200 DEG C with same heating rate, is naturally cooling to 1050 DEG C, heat preservation sintering 1h, nature
Demoulding obtains low magnetic loss magnetic material after being cooled to room temperature.
Example 2
It takes 105g pyrolusite stones to be placed in pulverizer to crush, sieves with 100 mesh sieve to obtain pyrolusite powder, pyrolusite powder is placed in reaction kettle
In, to the concentrated sulfuric acid solution and 25g orange peels that 45g iron powders are added in reaction kettle, 250mL mass fractions are 45%, it is stirred
After 25min, reaction kettle is moved into water-bath, is heated to 52 DEG C, insulation reaction 2.5h, filtering removal filter residue is soaked
Go out liquid；75g manganese dioxide is added into above-mentioned leachate, is heated to 85 DEG C, reacts 2.5h, obtains Oxidation Leaching liquid, after
Continuing the addition 35g manganese carbonates into Oxidation Leaching liquid, stirring filters Oxidation Leaching liquid until bubble generation, collects filtrate,
Filtrate is transferred in beaker, the ammonium hydroxide that mass fraction is 25% is added into beaker, it is 6.7 to adjust pH, is filtered after stirring 7min
Isolated deep iron removal liquid；The ammonium sulfide solution that 110mL mass fractions are 20%, heat temperature raising are added into deep iron removal liquid
To 75 DEG C, start magnetic stirring apparatus, after being stirred to react 1.5h with the rotating speed of 220r/min, stand 2 days, filtering removal flocculate obtains
To clarified solution, 9g ammonium fluorides are continuously added into clarified solution, are heated to 85 DEG C, are stirred to react 47min, after being purified
Manganese sulfate solution；The above-mentioned manganese sulfate solutions of 320mL are placed in beaker, 75mL absolute ethyl alcohols are added to beaker, then with ammonium hydroxide tune
It saves pH value of solution in beaker to move into water-bath beaker to 6.7, be heated to 77 DEG C, simultaneously with the rotating speed stirring of 750r/min
Air is passed through with air blower into beaker with the rate of 25L/min to pour into solution in beaker after insulated and stirred reacts 42min
In evaporating dish, 125 DEG C are heated to, evaporates 1.5h, purification obtains manganese compound；Iron oxide, zinc oxide, above-mentioned manganese compound are pressed
Mass ratio is 5 ︰ 1 ︰ 3 mixing, obtains mixture grind, by mixture grind and mass fraction for 25% poly-vinyl alcohol solution by
Mass ratio is that 1 ︰ 3 is mixed to get suspension, and suspension is put into ball mill, then it is 20 to press ball material mass ratio:1 into ball mill
The ball milling pearl that grain size is 0.2mm is added, ball milling 17h obtains magnetic core slurry；Magnetic core slurry is poured into cylindrical die, by mould
After tool is put into forcing press the compacting of the pressure with 7MPa 7min, mold is put into resistance furnace, is warming up to the rate of 2 DEG C/min
1070 DEG C, heat preservation sintering 2.5h, after continuation rises to 1220 DEG C with same heating rate, 1070 DEG C are naturally cooling to, heat preservation is burnt
1.5h is tied, is demoulded after cooled to room temperature and obtains low magnetic loss magnetic material.
Example 3
It takes 110g pyrolusite stones to be placed in pulverizer to crush, sieves with 100 mesh sieve to obtain pyrolusite powder, pyrolusite powder is placed in reaction kettle
In, to the concentrated sulfuric acid solution and 30g orange peels that 50g iron powders are added in reaction kettle, 300mL mass fractions are 45%, it is stirred
After 30min, reaction kettle is moved into water-bath, is heated to 55 DEG C, insulation reaction 3h, filtering removal filter residue is leached
Liquid；80g manganese dioxide is added into above-mentioned leachate, is heated to 90 DEG C, reacts 3h, obtains Oxidation Leaching liquid, continue to
40g manganese carbonates are added in Oxidation Leaching liquid, stirring filters Oxidation Leaching liquid until bubble generation, collects filtrate, will filter
Liquid is transferred in beaker, and the ammonium hydroxide that mass fraction is 25% is added into beaker, and it is 7.0 to adjust pH, stirs filtering point after 10min
From obtaining deep iron removal liquid；The ammonium sulfide solution that 120mL mass fractions are 20% is added into deep iron removal liquid, is heated to
80 DEG C, start magnetic stirring apparatus, after being stirred to react 2h with the rotating speed of 250r/min, stand 3 days, filtering removal flocculate obtains clear
Clear liquid continuously adds 10g ammonium fluorides into clarified solution, is heated to 90 DEG C, is stirred to react 50min, the sulphur after being purified
Sour manganese solution；The above-mentioned manganese sulfate solutions of 350mL are placed in beaker, 80mL absolute ethyl alcohols are added to beaker, then adjusted with ammonium hydroxide
Beaker is moved into water-bath to 6.8, is heated to 80 DEG C, is stirred and be used in combination with the rotating speed of 800r/min by pH value of solution in beaker
Air blower is passed through air with the rate of 30L/min into beaker and solution in beaker is poured into steaming after insulated and stirred reacts 45min
It sends out in ware, is heated to 130 DEG C, evaporate 2h, purification obtains manganese compound；Iron oxide, zinc oxide, above-mentioned manganese compound are pressed into quality
Than being mixed for 5 ︰, 1 ︰ 3, obtain mixture grind, by mixture grind and mass fraction for 25% poly-vinyl alcohol solution by quality
Than being mixed to get suspension for 1 ︰ 3, suspension is put into ball mill, then it is 20 to press ball material mass ratio:1 is added into ball mill
Grain size is the ball milling pearl of 0.3mm, and ball milling 20h obtains magnetic core slurry；Magnetic core slurry is poured into cylindrical die, mold is put
After entering the pressure compacting 8min in forcing press with 8MPa, mold is put into resistance furnace, 1100 are warming up to the rate of 3 DEG C/min
DEG C, heat preservation sintering 3h is naturally cooling to 1100 DEG C, heat preservation sintering 2h after continuation rises to 1250 DEG C with same heating rate, from
Demoulding obtains low magnetic loss magnetic material after being so cooled to room temperature.
Comparative example
With the low magnetic loss magnetic material of Suzhou company production as a comparison case to low magnetic loss magnetism material produced by the present invention
Low magnetic loss magnetic material in material and comparative example carries out performance detection, and testing result is as shown in table 1：
Test method：
Coercivity test is detected by GB/3656-2008 standards；
Power attenuation test is detected using magnetic material power consumption power inductance tester；
Magnetic permeability test is detected using magnetic permeability analyzer；
Saturation flux density clicks formula and is calculated：
Bs(T)=Bs(0)×(ρ/ρt)×(1-T/Tc)a
Wherein Bs (0) is the saturation flux density on 0 (K)；ρ/ρ t are density/theoretical density；Tc is Curie temperature.
1 magnetic material performance measurement result of table
Low according to the low magnetic loss magnetic material power attenuation produced by the present invention of data among the above, magnetic permeability is high, is saturated magnetic
Flux density is high, has broad application prospects.
Claims (7)
1. a kind of preparation method of low magnetic loss magnetic material, it is characterised in that specifically preparation process is：
（1）It takes 100~110g pyrolusite stones to be placed in pulverizer to crush, sieving obtains pyrolusite powder, and pyrolusite powder is placed in instead
It answers in kettle, 40~50g iron powders, 200~300mL concentrated sulfuric acid solutions and 20~30g orange peels is added to reaction kettle, is stirred
Afterwards, reaction kettle is moved into water-bath, heat temperature raising, insulation reaction, filtering removal filter residue obtains leachate；
（2）Into above-mentioned leachate be added 70~80g manganese dioxide, heat temperature raising, reaction, obtain Oxidation Leaching liquid, continue to
30~40g manganese carbonates are added in Oxidation Leaching liquid, stirring filters Oxidation Leaching liquid until bubble generation, collects filtrate,
Filtrate is transferred in beaker, ammonium hydroxide is added into beaker, adjusts pH, is separated by filtration to obtain deep iron removal after stirring 5~10min
Liquid；
（3）100~120mL ammonium sulfide solutions are added into deep iron removal liquid, heat temperature raising starts magnetic stirring apparatus, with 200~
After the rotating speed of 250r/min is stirred to react, standing, filtering removal flocculate obtains clarified solution, continuously add 8 into clarified solution~
10g ammonium fluorides, heat temperature raising are stirred to react, the manganese sulfate solution after being purified；
（4）The above-mentioned manganese sulfate solutions of 300~350mL are placed in beaker, 70~80mL absolute ethyl alcohols are added to beaker, then use ammonia
Water adjusts pH value of solution in beaker, and beaker is moved into water-bath, is heated to 75~80 DEG C, with turning for 700~800r/min
Speed stirs and is passed through air into beaker after insulated and stirred reaction with air blower and pours into solution in beaker in evaporating dish, heats
Heating, evaporation, purification obtain manganese compound；
（5）Iron oxide, zinc oxide, above-mentioned manganese compound are mixed, mixture to be ground is obtained, mixture to be ground and polyvinyl alcohol is molten
Liquid is mixed to get suspension, and suspension is put into ball mill, then ball milling pearl is added into ball mill by certain ball material mass ratio,
Ball milling obtains magnetic core slurry；
（6）Magnetic core slurry is poured into cylindrical die, mold is put into after suppressing 5~8min in forcing press, mold is put into
It is sintered in resistance furnace, is demoulded after cooled to room temperature and obtain low magnetic loss magnetic material.
2. a kind of preparation method of low magnetic loss magnetic material according to claim 1, it is characterised in that：Step（1）Institute
The be sieved specification stated is 100 mesh, and the mass fraction of concentrated sulfuric acid solution is 45%, and it is 20~30min, heating to be stirred the time
Temperature is 50~55 DEG C after heating, and the insulation reaction time is 2~3h.
3. a kind of preparation method of low magnetic loss magnetic material according to claim 1, it is characterised in that：Step（2）Institute
After the heat temperature raising stated temperature be 80~90 DEG C, the reaction time be 2~3h, ammonium hydroxide mass fraction be 25%, adjust pH be 6.5~
7.0。
4. a kind of preparation method of low magnetic loss magnetic material according to claim 1, it is characterised in that：Step（3）Institute
The mass fraction for the ammonium sulfide solution stated is 20%, is heated to 70~80 DEG C, and it is 1~2h, time of repose to be stirred to react the time
It it is 2~3 days, temperature is 80~90 DEG C after heat temperature raising, and it is 45~50min to be stirred to react the time.
5. a kind of preparation method of low magnetic loss magnetic material according to claim 1, it is characterised in that：Step（4）Institute
It is 6.5~6.8 that the ammonium hydroxide stated, which adjusts pH value of solution in beaker, and temperature is 75~80 DEG C after heat temperature raising, and air blower leads into beaker
It is 20~30L/min to enter air speed, and the insulated and stirred reaction time is 40~45min, and temperature is 120 after evaporating dish heat temperature raising
~130 DEG C, evaporation time is 1~2h.
6. a kind of preparation method of low magnetic loss magnetic material according to claim 1, it is characterised in that：Step（5）Institute
Iron oxide, zinc oxide, the manganese compound mixing quality ratio stated are 5 ︰, 1 ︰ 3, and mixture to be ground is in mass ratio with poly-vinyl alcohol solution
1 ︰ 3, poly-vinyl alcohol solution mass fraction are 25%, and ball material mass ratio is 20:1, ball milling bead diameter is 0.1~0.3mm, when ball milling
Between be 15~20h.
7. a kind of preparation method of low magnetic loss magnetic material according to claim 1, it is characterised in that：Step（6）Institute
The pressing pressure stated is 6~8MPa, and sintering process is：The rate of 2~3 DEG C/min is warming up to 1050~1100 DEG C, heat preservation sintering 2
~3h is naturally cooling to 1050~1100 DEG C, heat preservation sintering 1 after continuation rises to 1200~1250 DEG C with same heating rate
~2h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112086282A (en) * | 2020-07-27 | 2020-12-15 | 电子科技大学 | Manufacturing method and structure of miniaturized three-dimensional inductor with magnetic core |
| CN112951579A (en) * | 2021-01-29 | 2021-06-11 | 佛山市中研非晶科技股份有限公司 | Heat treatment method for residual magnetism of iron-based nanocrystalline magnetic core |
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|---|---|---|---|---|
| CN102070198A (en) * | 2011-02-28 | 2011-05-25 | 湖南科技大学 | Method for preparing high-purity manganese sulfate and high-purity manganese carbonate by reduction leaching of pyrolusite through scrap iron |
| CN107445209A (en) * | 2017-07-05 | 2017-12-08 | 四川大学 | Remove the method that manganous dithionate prepares saturation manganese sulfate slurries and manganese sulfate in pyrolusite pulp leachate |
| CN107827448A (en) * | 2017-11-21 | 2018-03-23 | 常州创索新材料科技有限公司 | A kind of preparation method of Mn-Zn soft magnetic ferrite |
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2018
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102070198A (en) * | 2011-02-28 | 2011-05-25 | 湖南科技大学 | Method for preparing high-purity manganese sulfate and high-purity manganese carbonate by reduction leaching of pyrolusite through scrap iron |
| CN107445209A (en) * | 2017-07-05 | 2017-12-08 | 四川大学 | Remove the method that manganous dithionate prepares saturation manganese sulfate slurries and manganese sulfate in pyrolusite pulp leachate |
| CN107827448A (en) * | 2017-11-21 | 2018-03-23 | 常州创索新材料科技有限公司 | A kind of preparation method of Mn-Zn soft magnetic ferrite |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112086282A (en) * | 2020-07-27 | 2020-12-15 | 电子科技大学 | Manufacturing method and structure of miniaturized three-dimensional inductor with magnetic core |
| CN112951579A (en) * | 2021-01-29 | 2021-06-11 | 佛山市中研非晶科技股份有限公司 | Heat treatment method for residual magnetism of iron-based nanocrystalline magnetic core |
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