CN106365623A - Wide-temperature broadband soft magnetic ferrite and preparation method of same - Google Patents
Wide-temperature broadband soft magnetic ferrite and preparation method of same Download PDFInfo
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- CN106365623A CN106365623A CN201610723995.3A CN201610723995A CN106365623A CN 106365623 A CN106365623 A CN 106365623A CN 201610723995 A CN201610723995 A CN 201610723995A CN 106365623 A CN106365623 A CN 106365623A
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- 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
- C04B35/2633—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 containing barium, strontium or calcium
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Abstract
The invention discloses wide-temperature broadband soft magnetic ferrite which is prepared from a main material and an auxiliary material according to the molar ratio of 1:(0.2-0.5), wherein the main material includes ferric oxide, zinc oxide and the balanced being silicon manganese powder, and on the basis of the weight of the main material, the auxiliary material includes calcium carbonate, zirconium oxide, niobium oxide, stannic oxide, cobalt oxide and molybdenum trioxide. The invention also discloses a preparation method of the wide-temperature broadband soft magnetic ferrite. The temperature range and frequency range of the soft magnetic ferrite can satisfy demand of daily use. The soft magnetic ferrite has high saturation magnetic flux density, high impedance, high Curie temperature and broad band.
Description
Technical field
The present invention relates to a kind of ferrite and preparation method thereof, more particularly, to a kind of broad temperature, broadband soft magnetic ferrite and its system
Preparation Method.
Background technology
With the fast development of digital communication technology and Fibre Optical Communication Technology, traditional artificial traffic equipment is continuously updated
Eliminate.In electronic circuit wide-band transformer, the pulse in the field such as ISDN(Integrated Service Digital Network), LAN, wide area network, background illumination becomes
The high magnetic permeability mnzn FERRITE CORE of common mode filtering inductance in depressor and photovoltaic DC-to-AC converter, because transformator etc. is towards small-sized
Change development, therefore requirements at the higher level have been put up to the magnetic characteristic of manganese-zinc ferrite, particularly in the Current electronic information age, extraneous ring
The various electronic interferences in border are increasingly serious, need manganese-zinc ferrite to have high initial permeability, high saturated magnetic induction, be in
In temperature, high impedance and broadband properties.
Demand when ferritic temperature range of the prior art and frequency range all cannot meet actually used, therefore
Need a kind of broad temperature, broadband soft magnetic ferrite of design badly to solve the problems of the prior art.
Content of the invention
For solving technical problem present in background technology, the present invention proposes a kind of broad temperature, broadband soft magnetic ferrite and its system
Preparation Method, the temperature range of the soft magnetic ferrite preparing and frequency range all can meet demand during routine use, have
The performance of high saturation magnetic flux density, high impedance, high-curie temperature and wideband.
A kind of broad temperature, broadband soft magnetic ferrite proposed by the present invention, is made up of major ingredient and adjuvant, major ingredient and adjuvant mole
Than for 1:(0.2-0.5), major ingredient is by mole inclusion: ferrum oxide 50.2-52.6mol%, zinc oxide 32.5-
36.5mol%, balance of silicomanganese powder；On the basis of the weight of major ingredient, adjuvant includes by weight percentage: Calcium Carbonate 0.02-
0.08wt%, zirconium oxide 0.03-0.05wt%, niobium oxide 0.020-0.040wt%, stannum oxide 0.15-0.18wt%, cobalt oxide
0.38-0.45wt%, molybdenum trioxide 0.32-0.36wt%.
Preferably, in described adjuvant, the percentage by weight of zirconium oxide and niobium oxide is 0.035-0.045:0.020-
0.040.
Preferably, in described adjuvant, cobalt oxide, the percentage by weight of molybdenum trioxide are 0.39-0.44:0.33-0.35.
Preferably, it is made up of major ingredient and adjuvant, the mol ratio of major ingredient and adjuvant is 1:(0.3-0.4), major ingredient presses moles hundred
Divide than inclusion: ferrum oxide 50.4-52.4mol%, zinc oxide 32.8-36.2mol%, balance of silicomanganese powder；Weight with major ingredient
On the basis of, adjuvant includes by weight percentage: Calcium Carbonate 0.03-0.07wt%, zirconium oxide 0.035-0.045wt%, niobium oxide
0.025-0.035wt%, stannum oxide 0.16-0.17wt%, cobalt oxide 0.39-0.44wt%, molybdenum trioxide 0.33-
0.35wt%.
Preferably, it is made up of major ingredient and adjuvant, the mol ratio of major ingredient and adjuvant is 1:0.35, and major ingredient is by mole bag
Include: ferrum oxide 51.4mol%, zinc oxide 34.5mol%, balance of silicomanganese powder；On the basis of the weight of major ingredient, adjuvant is by weight
Percentage ratio includes: Calcium Carbonate 0.05wt%, zirconium oxide 0.04wt%, niobium oxide 0.030wt%, stannum oxide 0.165wt%, oxidation
Cobalt 0.415wt%, molybdenum trioxide 0.34wt%.
A kind of preparation method of broad temperature, broadband soft magnetic ferrite proposed by the present invention, comprises the steps:
S1, major ingredient is carried out wet mixed, a ball milling 60-80min, then it is spray-dried, carry out pre-burning；
S2, in pre-burning major ingredient, add adjuvant, dispersant and defoamer mix homogeneously, carry out secondary ball milling 1-1.5h, obtain
To particle diameter for 0.8-1.2 micron powder；
Add organic bond mix homogeneously in s3, the powder obtaining to s2, mist projection granulating obtains particulate material, by particulate material in
50mpa-200mpa is pressed into green compact sample；
S4, the green compact sample obtaining s3 are warming up to 700-800 DEG C, are incubated 15-45min；It is warming up to 700-1200 DEG C, protect
Warm 25-45min, in temperature-rise period, partial pressure of oxygen maintains 1-2%；It is warming up to 1250-1350 DEG C, be incubated 2-9h, temperature-rise period
In, partial pressure of oxygen maintains 3-21%；It is cooled to 950-1050 DEG C, be incubated 2-5h；It is cooled to room temperature and obtain broad temperature, broadband soft magnet
Oxysome.
Preferably, in s1, calcined temperature is 850-900 DEG C, and burn-in time is 1-2h.
The present invention a kind of broad temperature, broadband soft magnetic ferrite, be made up by a certain percentage of major ingredient and adjuvant, major ingredient includes
Ferrum oxide, zinc oxide, balance of silicomanganese powder；On the basis of the weight of major ingredient, adjuvant includes: Calcium Carbonate, zirconium oxide, niobium oxide,
Stannum oxide, cobalt oxide and molybdenum trioxide.Mix homogeneously after major ingredient ferrum oxide, zinc oxide and the silicomanganese sphere of powder are ground, Ran Houjing
Cross pre-burning, be subsequently added into adjuvant Calcium Carbonate, zirconium oxide, niobium oxide, stannum oxide, cobalt oxide and molybdenum trioxide and carry out secondary ball milling,
Then it is sintered, the temperature range of the soft magnetic ferrite obtaining and frequency range all can meet demand during routine use, tool
There is the performance of high saturation magnetic flux density, high impedance, high-curie temperature and wideband.Wherein, pcrmeability is 7230, and Curie temperature is
185 DEG C, the impedance of 500khz-1mhz is 156 ω.
Specific embodiment
With reference to specific embodiment, the present invention is described in detail it should be appreciated that embodiment is served only for this is described
Bright, rather than be used for limiting the invention, any modification made on the basis of the present invention, equivalent etc. are all at this
In bright protection domain.
Embodiment 1
A kind of broad temperature, broadband soft magnetic ferrite proposed by the present invention, is made up of major ingredient and adjuvant, major ingredient and adjuvant mole
Than for 1:0.35, major ingredient is by mole inclusion: ferrum oxide 51.4mol%, zinc oxide 34.5mol%, balance of silicomanganese powder；
On the basis of the weight of major ingredient, adjuvant includes by weight percentage: Calcium Carbonate 0.05wt%, zirconium oxide 0.04wt%, niobium oxide
0.030wt%, stannum oxide 0.165wt%, cobalt oxide 0.415wt%, molybdenum trioxide 0.34wt%.
Embodiment 2
A kind of broad temperature, broadband soft magnetic ferrite proposed by the present invention, is made up of major ingredient and adjuvant, major ingredient and adjuvant mole
Than for 1:0.2, major ingredient is by mole inclusion: ferrum oxide 50.2mol%, zinc oxide 36.5mol%, balance of silicomanganese powder；
On the basis of the weight of major ingredient, adjuvant includes by weight percentage: Calcium Carbonate 0.02wt%, zirconium oxide 0.05wt%, niobium oxide
0.020wt%, stannum oxide 0.18wt%, cobalt oxide 0.38wt%, molybdenum trioxide 0.36wt%.
A kind of preparation method of broad temperature, broadband soft magnetic ferrite proposed by the present invention, comprises the steps:
S1, major ingredient is carried out wet mixed, a ball milling 60min, then it is spray-dried, carries out pre-burning, calcined temperature is
900 DEG C, burn-in time is 1h；
S2, in pre-burning major ingredient, add adjuvant, dispersant and defoamer mix homogeneously, carry out secondary ball milling 1h, obtain grain
Footpath is 1.2 microns of powder；
Add organic bond mix homogeneously in s3, the powder obtaining to s2, mist projection granulating obtains particulate material, by particulate material in
50mpa is pressed into green compact sample；
S4, the green compact sample obtaining s3 are warming up to 800 DEG C, are incubated 15min；It is warming up to 1200 DEG C, is incubated 25min, rise
During temperature, partial pressure of oxygen maintains 2%；It is warming up to 1250 DEG C, be incubated 9h, in temperature-rise period, partial pressure of oxygen maintains 3%；Cooling
To 1050 DEG C, it is incubated 2h；It is cooled to room temperature and obtain broad temperature, broadband soft magnetic ferrite.
Embodiment 3
A kind of broad temperature, broadband soft magnetic ferrite proposed by the present invention, is made up of major ingredient and adjuvant, major ingredient and adjuvant mole
Than for 1:0.5, major ingredient is by mole inclusion: ferrum oxide 52.6mol%, zinc oxide 32.5mol%, balance of silicomanganese powder；
On the basis of the weight of major ingredient, adjuvant includes by weight percentage: Calcium Carbonate 0.08wt%, zirconium oxide 0.03wt%, niobium oxide
0.040wt%, stannum oxide 0.15wt%, cobalt oxide 0.45wt%, molybdenum trioxide 0.32wt%.
A kind of preparation method of broad temperature, broadband soft magnetic ferrite proposed by the present invention, comprises the steps:
S1, major ingredient is carried out wet mixed, a ball milling 80min, then it is spray-dried, carries out pre-burning, calcined temperature is
850 DEG C, burn-in time is 2h；
S2, in pre-burning major ingredient, add adjuvant, dispersant and defoamer mix homogeneously, carry out secondary ball milling 1h, obtain grain
Footpath is 1.2 microns of powder；
Add organic bond mix homogeneously in s3, the powder obtaining to s2, mist projection granulating obtains particulate material, by particulate material in
50mpa is pressed into green compact sample；
S4, the green compact sample obtaining s3 are warming up to 800 DEG C, are incubated 15min；It is warming up to 1200 DEG C, is incubated 25min, rise
During temperature, partial pressure of oxygen maintains 2%；It is warming up to 1250 DEG C, be incubated 9h, in temperature-rise period, partial pressure of oxygen maintains 3%；Cooling
To 1050 DEG C, it is incubated 2h；It is cooled to room temperature and obtain broad temperature, broadband soft magnetic ferrite.
Embodiment 4
A kind of broad temperature, broadband soft magnetic ferrite proposed by the present invention, is made up of major ingredient and adjuvant, major ingredient and adjuvant mole
Than for 1:0.3, major ingredient is by mole inclusion: ferrum oxide 50.4mol%, zinc oxide 36.2mol%, balance of silicomanganese powder；
On the basis of the weight of major ingredient, adjuvant includes by weight percentage: Calcium Carbonate 0.03wt%, zirconium oxide 0.045wt%, niobium oxide
0.025wt%, stannum oxide 0.17wt%, cobalt oxide 0.39wt%, molybdenum trioxide 0.35wt%.
A kind of preparation method of broad temperature, broadband soft magnetic ferrite proposed by the present invention, comprises the steps:
S1, major ingredient is carried out wet mixed, a ball milling 65min, then it is spray-dried, carries out pre-burning, calcined temperature is
890 DEG C, burn-in time is 1.2h；
S2, in pre-burning major ingredient, add adjuvant, dispersant and defoamer mix homogeneously, carry out secondary ball milling 1.4h, obtain
Particle diameter is 0.9 micron of powder；
Add organic bond mix homogeneously in s3, the powder obtaining to s2, mist projection granulating obtains particulate material, by particulate material in
190mpa is pressed into green compact sample；
S4, the green compact sample obtaining s3 are warming up to 720 DEG C, are incubated 42min；It is warming up to 800 DEG C, is incubated 42min, heat up
During, partial pressure of oxygen maintains 1.2%；It is warming up to 1320 DEG C, be incubated 3h, in temperature-rise period, partial pressure of oxygen maintains 20%；Cooling
To 980 DEG C, it is incubated 4h；It is cooled to room temperature and obtain broad temperature, broadband soft magnetic ferrite.
Embodiment 5
A kind of broad temperature, broadband soft magnetic ferrite proposed by the present invention, is made up of major ingredient and adjuvant, major ingredient and adjuvant mole
Than for 1:0.4, major ingredient is by mole inclusion: ferrum oxide 52.4mol%, zinc oxide 32.8mol%, balance of silicomanganese powder；
On the basis of the weight of major ingredient, adjuvant includes by weight percentage: Calcium Carbonate 0.07wt%, zirconium oxide 0.035wt%, niobium oxide
0.035wt%, stannum oxide 0.16wt%, cobalt oxide 0.44wt%, molybdenum trioxide 0.33wt%.
A kind of preparation method of broad temperature, broadband soft magnetic ferrite proposed by the present invention, comprises the steps:
S1, major ingredient is carried out wet mixed, a ball milling 75min, then it is spray-dried, carries out pre-burning, calcined temperature is
860 DEG C, burn-in time is 1.8h；
S2, in pre-burning major ingredient, add adjuvant, dispersant and defoamer mix homogeneously, carry out secondary ball milling 1.1h, obtain
Particle diameter is 1.1 microns of powder；
Add organic bond mix homogeneously in s3, the powder obtaining to s2, mist projection granulating obtains particulate material, by particulate material in
60mpa is pressed into green compact sample；
S4, the green compact sample obtaining s3 are warming up to 780 DEG C, are incubated 18min；It is warming up to 1100 DEG C, is incubated 28min, rise
During temperature, partial pressure of oxygen maintains 1.8%；It is warming up to 1280 DEG C, be incubated 8h, in temperature-rise period, partial pressure of oxygen maintains 4%；Fall
Temperature, to 1020 DEG C, is incubated 3h；It is cooled to room temperature and obtain broad temperature, broadband soft magnetic ferrite.
The inductance value of different temperatures and frequency sample during test, is measured using hp4294a electric impedance analyzer and special fixture
L, calculates corresponding initial permeability ui and Curie temperature, and uses 0.35mm single-turn circular coil at normal temperatures in 0.02v voltage
Measure its frequency characteristic；To sample elder generation sanding and polishing, with ethanol, acetone, surface clean is clean, it is then coated with silver paste, then with two
Piece copper coin clamps, and dries at 100 DEG C, measures sample under different frequency (100khz-1mhz) with hp4294a electric impedance analyzer
Resistance, calculates the frequency characteristic of sample resistivity pe.Embodiment result is listed in table 1 below.
Table 1:
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any those familiar with the art the invention discloses technical scope in, technology according to the present invention scheme and its
Inventive concept equivalent or change in addition, all should be included within the scope of the present invention.
Claims (7)
1. it is characterised in that being made up of major ingredient and adjuvant, the mol ratio of major ingredient and adjuvant is a kind of broad temperature, broadband soft magnetic ferrite
1:(0.2-0.5), major ingredient is by mole inclusion: ferrum oxide 50.2-52.6mol%, zinc oxide 32.5-36.5mol%, remaining
Measure as silicomanganese powder；On the basis of the weight of major ingredient, adjuvant includes by weight percentage: Calcium Carbonate 0.02-0.08wt%, zirconium oxide
0.03-0.05wt%, niobium oxide 0.020-0.040wt%, stannum oxide 0.15-0.18wt%, cobalt oxide 0.38-0.45wt%,
Molybdenum trioxide 0.32-0.36wt%.
2. broad temperature, broadband soft magnetic ferrite according to claim 1 is it is characterised in that in described adjuvant, zirconium oxide and oxygen
The percentage by weight changing niobium is 0.035-0.045:0.020-0.040.
3. broad temperature, broadband soft magnetic ferrite according to claim 1 and 2 is it is characterised in that in described adjuvant, cobalt oxide,
The percentage by weight of molybdenum trioxide is 0.39-0.44:0.33-0.35.
4. the broad temperature, broadband soft magnetic ferrite according to any one of claim 1-3 is it is characterised in that by major ingredient and adjuvant system
Become, the mol ratio of major ingredient and adjuvant is 1:(0.3-0.4), major ingredient is by mole inclusion: ferrum oxide 50.4-52.4mol%,
Zinc oxide 32.8-36.2mol%, balance of silicomanganese powder；On the basis of the weight of major ingredient, adjuvant includes by weight percentage: carbon
Sour calcium 0.03-0.07wt%, zirconium oxide 0.035-0.045wt%, niobium oxide 0.025-0.035wt%, stannum oxide 0.16-
0.17wt%, cobalt oxide 0.39-0.44wt%, molybdenum trioxide 0.33-0.35wt%.
5. the broad temperature, broadband soft magnetic ferrite according to any one of claim 1-4 is it is characterised in that by major ingredient and adjuvant system
Become, the mol ratio of major ingredient and adjuvant is 1:0.35, and major ingredient is by mole inclusion: ferrum oxide 51.4mol%, zinc oxide
34.5mol%, balance of silicomanganese powder；On the basis of the weight of major ingredient, adjuvant includes by weight percentage: Calcium Carbonate
0.05wt%, zirconium oxide 0.04wt%, niobium oxide 0.030wt%, stannum oxide 0.165wt%, cobalt oxide 0.415wt%, three oxygen
Change molybdenum 0.34wt%.
6. the broad temperature, broadband soft magnetic ferrite described in a kind of any one according to claim 1-5 preparation method it is characterised in that
Comprise the steps:
S1, major ingredient is carried out wet mixed, a ball milling 60-80min, then it is spray-dried, carry out pre-burning；
S2, in pre-burning major ingredient, add adjuvant, dispersant and defoamer mix homogeneously, carry out secondary ball milling 1-1.5h, obtain grain
Footpath is the powder of 0.8-1.2 micron；
Add organic bond mix homogeneously in s3, the powder obtaining to s2, mist projection granulating obtains particulate material, by particulate material in
50mpa-200mpa is pressed into green compact sample；
S4, the green compact sample obtaining s3 are warming up to 700-800 DEG C, are incubated 15-45min；It is warming up to 700-1200 DEG C, insulation
25-45min, in temperature-rise period, partial pressure of oxygen maintains 1-2%；It is warming up to 1250-1350 DEG C, be incubated 2-9h, in temperature-rise period,
Partial pressure of oxygen maintains 3-21%；It is cooled to 950-1050 DEG C, be incubated 2-5h；It is cooled to room temperature and obtain broad temperature, broadband soft magnet oxygen
Body.
7. the preparation method of broad temperature, broadband soft magnetic ferrite according to claim 6 is it is characterised in that in s1, pre-burning temperature
Spend for 850-900 DEG C, burn-in time is 1-2h.
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