CN106348742A - Soft magnetic ferrite material with high magnetic conductivity and low temperature coefficient and preparation method thereof - Google Patents

Soft magnetic ferrite material with high magnetic conductivity and low temperature coefficient and preparation method thereof Download PDF

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Publication number
CN106348742A
CN106348742A CN201610719250.XA CN201610719250A CN106348742A CN 106348742 A CN106348742 A CN 106348742A CN 201610719250 A CN201610719250 A CN 201610719250A CN 106348742 A CN106348742 A CN 106348742A
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oxide
soft magnetic
low temperature
raw material
magnetic ferrite
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瞿德林
王久如
李丛俊
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TIANCHANG ZHONGDE ELECTRONICS CO Ltd
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TIANCHANG ZHONGDE ELECTRONICS CO Ltd
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    • C04B35/2608Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead
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Abstract

The invention discloses a soft magnetic ferrite material with high magnetic conductivity and low temperature coefficient. The soft magnetic ferrite material is prepared from the following raw materials: ferric oxide, nickel oxide, zinc oxide, manganese carbonate, cobaltic oxide, vanadium oxide, tin dioxide, aluminum oxide, tungsten trioxide, chromium oxide and a composite sintering agent; and a polyvinyl alcohol aqueous solution and zinc stearate, wherein the content of the polyvinyl alcohol aqueous solution accounts for 3 to 5 percent of the total amount of the raw materials, and the content of the zinc stearate accounts for 0.5 to 1.5 percent of the total amount of the raw materials. The invention also provides a preparation method of the soft magnetic ferrite material with high magnetic conductivity and low temperature coefficient. The soft magnetic ferrite material prepared by the method is high in magnetic conductivity and low in temperature coefficient.

Description

A kind of soft magnetic ferrite of high magnetoconductivity low temperature degree coefficient and preparation method thereof
Technical field
The present invention relates to a kind of soft magnetic ferrite and preparation method thereof, more particularly, to a kind of high magnetoconductivity low temperature degree system Soft magnetic ferrite of number and preparation method thereof.
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 conductivity ferrite magnetic core of common mode filtering inductance in depressor and photovoltaic DC-to-AC converter, because transformator etc. is sent out towards miniaturization Exhibition, therefore requirements at the higher level are proposed to ferritic magnetic characteristic, particularly in the Current electronic information age, external environment various Electronic interferences are increasingly serious, need ferrite to have high initial permeability, high saturated magnetic induction, high-curie temperature, high resistant Resist and broadband properties.
The pcrmeability of soft magnetic ferrite of the prior art and temperature coefficient cannot meet the demand of prior art, therefore urgently A kind of soft magnetic ferrite of high magnetoconductivity low temperature degree coefficient need to be designed 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 soft magnetism of high magnetoconductivity low temperature degree coefficient Ferrite Material and preparation method thereof, the soft magnetic ferrite pcrmeability preparing is high, and temperature coefficient is low.
A kind of soft magnetic ferrite of high magnetoconductivity low temperature degree coefficient proposed by the present invention, molar part bag pressed by its raw material Include: ferrum oxide 48.5-52.5 part, nickel oxide 16.5-19.5 part, zinc oxide 14.6-18.2 part, manganese carbonate 2.8-3.6 part, three oxygen Change two cobalt 0.35-0.55 parts, vanadium oxide 0.05-0.15 part, tin ash 0.01-0.05 part, aluminium sesquioxide 0.005-0.015 Part, titanium dioxide 0.04-0.06 part, Tungstic anhydride. 0.02-0.04 part, chromium oxide 0.05-0.15 part, Composite sintering agent 0.25- 0.45 part;
Polyvinyl alcohol water solution and zinc stearate, the content of polyvinyl alcohol water solution accounts for the 3-5wt% of raw material total amount, Hard Fat The content of sour zinc accounts for the 0.5-1.5wt% of raw material total amount.
Preferably, Composite sintering agent is by calcium fluoride, Calcium Carbonate, silicon dioxide, copper oxide, bismuth oxide and vanadium oxide by weight Mix than 1-3:2-5:3-6:1-4:3-8:2-6.
Preferably, in Composite sintering agent raw material, Calcium Carbonate adopts purity more than 99%, and granularity is less than the fine powder of 320 mesh.
Preferably, in Composite sintering agent raw material, the purity more than 94% of silicon dioxide, particle mean size is less than 1 μm.
Preferably, its raw material is included by molar part: ferrum oxide 49.5-51.5 part, nickel oxide 17.5-18.5 part, zinc oxide 15.6-17.2 part, manganese carbonate 2.9-3.5 part, cobalt sesquioxide 0.38-0.52 part, vanadium oxide 0.08-0.12 part, tin ash 0.02-0.04 part, aluminium sesquioxide 0.008-0.012 part, titanium dioxide 0.045-0.055 part, Tungstic anhydride. 0.025-0.035 Part, chromium oxide 0.08-0.12 part, Composite sintering agent 0.28-0.42 part;
Polyvinyl alcohol water solution and zinc stearate, the content of polyvinyl alcohol water solution accounts for the 3.5-4.5wt% of raw material total amount, The content of zinc stearate accounts for the 0.8-1.2wt% of raw material total amount.
Preferably, its raw material is included by molar part: 50.5 parts of ferrum oxide, 18.0 parts of nickel oxide, 16.4 parts of zinc oxide, carbonic acid 3.2 parts of manganese, 0.45 part of cobalt sesquioxide, 0.10 part of vanadium oxide, 0.03 part of tin ash, 0.010 part of aluminium sesquioxide, titanium dioxide 0.05 part of titanium, 0.03 part of Tungstic anhydride., 0.10 part of chromium oxide, 0.35 part of Composite sintering agent;
Polyvinyl alcohol water solution and zinc stearate, the content of polyvinyl alcohol water solution accounts for the 4wt% of raw material total amount, stearic acid The content of zinc accounts for the 1.0wt% of raw material total amount.
A kind of preparation method of the soft magnetic ferrite of high magnetoconductivity low temperature degree coefficient proposed by the present invention, including as follows Step:
S1, mixing: ferrum oxide, nickel oxide, zinc oxide, manganese carbonate and cobalt sesquioxide are put into vibromill in vibrating mill 1-2h, makes dispensing be sufficiently mixed and obtains material a;
S2, pre-burning: material a is carried out in pushed bat kiln pre-burning and obtain material b;
S3, pulverizing: add vanadium oxide, tin ash, aluminium sesquioxide, titanium dioxide, Tungstic anhydride. and oxygen in material b Carry out waterproof pulverization after changing chromium, be subsequently adding zinc stearate and Composite sintering agent mix homogeneously obtains material c;
S4, pelletize: add the polyvinyl alcohol water solution of the 1.6-2.2% being equivalent to material c weight in material c, adopt Mist projection granulating, obtains particulate material;
S5, compacting: the particulate material obtaining in s4 is obtained blank using powder former compacting;
S6, sintering: blank is put in resistance furnace and is sintered, sintering processes include: be warming up to 1200-1300 DEG C, it is incubated 10-30min, is then cooled to 1150-1180 DEG C, be incubated 2-4h, then 1280-1350 DEG C of intensification, be incubated 2-4h, Then naturally cool to the soft magnetic ferrite that room temperature obtains high magnetoconductivity low temperature degree coefficient.
Preferably, in s2, calcined temperature is 1000-1100 DEG C, and burn-in time is 2-4h.
A kind of soft magnetic ferrite of high magnetoconductivity low temperature degree coefficient of the present invention, its raw material includes ferrum oxide, oxidation Nickel, zinc oxide, manganese carbonate, cobalt sesquioxide, vanadium oxide, tin ash, aluminium sesquioxide, titanium dioxide, Tungstic anhydride., oxidation Chromium, Composite sintering agent;Polyvinyl alcohol water solution and zinc stearate, the content of polyvinyl alcohol water solution accounts for the 3- of raw material total amount 5wt%, the content of zinc stearate accounts for the 0.5-1.5wt% of raw material total amount.By ferrum oxide, nickel oxide, zinc oxide, manganese carbonate and three Aoxidize two cobalts and put into vibromill in vibrating mill, then carry out pre-burning, be subsequently added into vanadium oxide, tin ash, aluminium sesquioxide, Carry out waterproof pulverization after titanium dioxide, Tungstic anhydride. and chromium oxide, be subsequently adding zinc stearate and Composite sintering agent mix homogeneously, It is subsequently adding polyvinyl alcohol water solution and carries out pelletize, be pressed into blank after obtaining particulate material, be finally sintered, be cooled to Room temperature obtains the soft magnetic ferrite of the high magnetoconductivity low temperature degree coefficient of the present invention, and wherein Composite sintering agent is by calcium fluoride, carbon Sour calcium, silicon dioxide, copper oxide, bismuth oxide and vanadium oxide mix, and the titanium dioxide adding wherein in raw material can be in crystal boundary With calcium titanium-type resistive formation, ti4+Ion increase causes fe3+Ion reduces, fe2+Content increases, and controls fe2+Content just can adjust two Peak position, ti4+And co2+The synergy of ion, forces down " hump " and can receive excellent effect, so ferritic temperature model Enclose and be compensated regulation, be conducive to obtaining the wide temperature characteristics of material.The soft magnetic ferrite pcrmeability that the present invention prepares Height, temperature coefficient is low.
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 soft magnetic ferrite of high magnetoconductivity low temperature degree coefficient proposed by the present invention, molar part bag pressed by its raw material Include: 50.5 parts of ferrum oxide, 18.0 parts of nickel oxide, 16.4 parts of zinc oxide, 3.2 parts of manganese carbonate, 0.45 part of cobalt sesquioxide, vanadium oxide 0.10 part, 0.03 part of tin ash, 0.010 part of aluminium sesquioxide, 0.05 part of titanium dioxide, 0.03 part of Tungstic anhydride., chromium oxide 0.10 part, 0.35 part of Composite sintering agent;
Polyvinyl alcohol water solution and zinc stearate, the content of polyvinyl alcohol water solution accounts for the 4wt% of raw material total amount, stearic acid The content of zinc accounts for the 1.0wt% of raw material total amount.
Embodiment 2
A kind of soft magnetic ferrite of high magnetoconductivity low temperature degree coefficient proposed by the present invention, molar part bag pressed by its raw material Include: 48.5 parts of ferrum oxide, 19.5 parts of nickel oxide, 14.6 parts of zinc oxide, 3.6 parts of manganese carbonate, 0.35 part of cobalt sesquioxide, vanadium oxide 0.15 part, 0.01 part of tin ash, 0.015 part of aluminium sesquioxide, 0.04 part of titanium dioxide, 0.04 part of Tungstic anhydride., chromium oxide 0.05 part, 0.45 part of Composite sintering agent;
Polyvinyl alcohol water solution and zinc stearate, the content of polyvinyl alcohol water solution accounts for the 3wt% of raw material total amount, stearic acid The content of zinc accounts for the 1.5wt% of raw material total amount.
Composite sintering agent is by calcium fluoride, Calcium Carbonate, silicon dioxide, copper oxide, bismuth oxide and vanadium oxide by weight 1:5: 3:4:3:6 mixes.
Embodiment 3
A kind of soft magnetic ferrite of high magnetoconductivity low temperature degree coefficient proposed by the present invention, molar part bag pressed by its raw material Include: 52.5 parts of ferrum oxide, 16.5 parts of nickel oxide, 18.2 parts of zinc oxide, 2.8 parts of manganese carbonate, 0.55 part of cobalt sesquioxide, vanadium oxide 0.05 part, 0.05 part of tin ash, 0.005 part of aluminium sesquioxide, 0.06 part of titanium dioxide, 0.02 part of Tungstic anhydride., chromium oxide 0.15 part, 0.25 part of Composite sintering agent;
Polyvinyl alcohol water solution and zinc stearate, the content of polyvinyl alcohol water solution accounts for the 5wt% of raw material total amount, stearic acid The content of zinc accounts for the 0.5wt% of raw material total amount.
Composite sintering agent is by calcium fluoride, Calcium Carbonate, silicon dioxide, copper oxide, bismuth oxide and vanadium oxide by weight 3:2: 6:1:8:2 mixes.
A kind of preparation method of the soft magnetic ferrite of high magnetoconductivity low temperature degree coefficient proposed by the present invention, including as follows Step:
S1, mixing: ferrum oxide, nickel oxide, zinc oxide, manganese carbonate and cobalt sesquioxide are put into vibromill in vibrating mill 2h, makes dispensing be sufficiently mixed and obtains material a;
S2, pre-burning: material a is carried out in pushed bat kiln pre-burning and obtain material b, calcined temperature is 1000 DEG C, burn-in time For 4h;
S3, pulverizing: add vanadium oxide, tin ash, aluminium sesquioxide, titanium dioxide, Tungstic anhydride. and oxygen in material b Carry out waterproof pulverization after changing chromium, be subsequently adding zinc stearate and Composite sintering agent mix homogeneously obtains material c;
S4, pelletize: add be equivalent to material c weight 1.6% polyvinyl alcohol water solution in material c, using spraying Pelletize, obtains particulate material;
S5, compacting: the particulate material obtaining in s4 is obtained blank using powder former compacting;
S6, sintering: blank is put in resistance furnace and is sintered, sintering processes include: be warming up to 1300 DEG C, insulation 10min, is then cooled to 1180 DEG C, is incubated 2h, then heats up 1350 DEG C, is incubated 2h, then naturally cools to room temperature and obtain height The soft magnetic ferrite of magnetoconductivity low temperature degree coefficient.
Embodiment 4
A kind of soft magnetic ferrite of high magnetoconductivity low temperature degree coefficient proposed by the present invention, molar part bag pressed by its raw material Include: 49.5 parts of ferrum oxide, 18.5 parts of nickel oxide, 15.6 parts of zinc oxide, 3.5 parts of manganese carbonate, 0.38 part of cobalt sesquioxide, vanadium oxide 0.12 part, 0.02 part of tin ash, 0.012 part of aluminium sesquioxide, 0.045 part of titanium dioxide, 0.035 part of Tungstic anhydride., oxidation 0.08 part of chromium, 0.42 part of Composite sintering agent;
Polyvinyl alcohol water solution and zinc stearate, the content of polyvinyl alcohol water solution accounts for the 3.5wt% of raw material total amount, Hard Fat The content of sour zinc accounts for the 1.2wt% of raw material total amount.
Composite sintering agent is by calcium fluoride, Calcium Carbonate, silicon dioxide, copper oxide, bismuth oxide and vanadium oxide by weight 1.5: 4:4:3:4:5 mixes.
A kind of preparation method of the soft magnetic ferrite of high magnetoconductivity low temperature degree coefficient proposed by the present invention, including as follows Step:
S1, mixing: ferrum oxide, nickel oxide, zinc oxide, manganese carbonate and cobalt sesquioxide are put into vibromill in vibrating mill 1.2-1.8h, makes dispensing be sufficiently mixed and obtains material a;
S2, pre-burning: material a is carried out in pushed bat kiln pre-burning and obtain material b, calcined temperature is 1020 DEG C, burn-in time For 3.5h;
S3, pulverizing: add vanadium oxide, tin ash, aluminium sesquioxide, titanium dioxide, Tungstic anhydride. and oxygen in material b Carry out waterproof pulverization after changing chromium, be subsequently adding zinc stearate and Composite sintering agent mix homogeneously obtains material c;
S4, pelletize: add be equivalent to material c weight 1.7% polyvinyl alcohol water solution in material c, using spraying Pelletize, obtains particulate material;
S5, compacting: the particulate material obtaining in s4 is obtained blank using powder former compacting;
S6, sintering: blank is put in resistance furnace and is sintered, sintering processes include: be warming up to 1280 DEG C, insulation 15min, is then cooled to 1175 DEG C, is incubated 2.5h, then heats up 1340 DEG C, is incubated 2.5h, then naturally cools to room temperature and obtain Soft magnetic ferrite to high magnetoconductivity low temperature degree coefficient.
Embodiment 5
A kind of soft magnetic ferrite of high magnetoconductivity low temperature degree coefficient proposed by the present invention, molar part bag pressed by its raw material Include: 51.5 parts of ferrum oxide, 17.5 parts of nickel oxide, 17.2 parts of zinc oxide, 2.9 parts of manganese carbonate, 0.52 part of cobalt sesquioxide, vanadium oxide 0.08 part, 0.04 part of tin ash, 0.008 part of aluminium sesquioxide, 0.055 part of titanium dioxide, 0.025 part of Tungstic anhydride., oxidation 0.12 part of chromium, 0.28 part of Composite sintering agent;
Polyvinyl alcohol water solution and zinc stearate, the content of polyvinyl alcohol water solution accounts for the 4.5wt% of raw material total amount, Hard Fat The content of sour zinc accounts for the 0.8wt% of raw material total amount.
Composite sintering agent is by calcium fluoride, Calcium Carbonate, silicon dioxide, copper oxide, bismuth oxide and vanadium oxide by weight 2.5: 3:5:2:7:3 mixes.
A kind of preparation method of the soft magnetic ferrite of high magnetoconductivity low temperature degree coefficient proposed by the present invention, including as follows Step:
S1, mixing: ferrum oxide, nickel oxide, zinc oxide, manganese carbonate and cobalt sesquioxide are put into vibromill in vibrating mill 1.8h, makes dispensing be sufficiently mixed and obtains material a;
S2, pre-burning: material a is carried out in pushed bat kiln pre-burning and obtain material b, calcined temperature is 1020 DEG C, burn-in time For 3.5h;
S3, pulverizing: add vanadium oxide, tin ash, aluminium sesquioxide, titanium dioxide, Tungstic anhydride. and oxygen in material b Carry out waterproof pulverization after changing chromium, be subsequently adding zinc stearate and Composite sintering agent mix homogeneously obtains material c;
S4, pelletize: add be equivalent to material c weight 1.7% polyvinyl alcohol water solution in material c, using spraying Pelletize, obtains particulate material;
S5, compacting: the particulate material obtaining in s4 is obtained blank using powder former compacting;
S6, sintering: blank is put in resistance furnace and is sintered, sintering processes include: be warming up to 1280 DEG C, insulation 15min, is then cooled to 1175 DEG C, is incubated 2.5h, then heats up 1340 DEG C, is incubated 2.5h, then naturally cools to room temperature and obtain Soft magnetic ferrite to high magnetoconductivity low temperature degree coefficient.
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 (8)

1. a kind of soft magnetic ferrite of high magnetoconductivity low temperature degree coefficient is it is characterised in that its raw material is included by molar part: oxygen Change ferrum 48.5-52.5 part, nickel oxide 16.5-19.5 part, zinc oxide 14.6-18.2 part, manganese carbonate 2.8-3.6 part, three oxidations two Cobalt 0.35-0.55 part, vanadium oxide 0.05-0.15 part, tin ash 0.01-0.05 part, aluminium sesquioxide 0.005-0.015 part, Titanium dioxide 0.04-0.06 part, Tungstic anhydride. 0.02-0.04 part, chromium oxide 0.05-0.15 part, Composite sintering agent 0.25-0.45 Part;
Polyvinyl alcohol water solution and zinc stearate, the content of polyvinyl alcohol water solution accounts for the 3-5wt% of raw material total amount, zinc stearate Content account for the 0.5-1.5wt% of raw material total amount.
2. the soft magnetic ferrite of high magnetoconductivity low temperature degree coefficient according to claim 1 is it is characterised in that compound burn Knot agent is by calcium fluoride, Calcium Carbonate, silicon dioxide, copper oxide, bismuth oxide and vanadium oxide by weight 1-3:2-5:3-6:1-4:3- 8:2-6 mixes.
3. the soft magnetic ferrite of high magnetoconductivity low temperature degree coefficient according to claim 1 and 2 is it is characterised in that answer Close in agglutinant raw material, Calcium Carbonate adopts purity more than 99%, granularity is less than the fine powder of 320 mesh.
4. the soft magnetic ferrite of the high magnetoconductivity low temperature degree coefficient according to any one of claim 1-3, its feature exists In, in Composite sintering agent raw material, the purity more than 94% of silicon dioxide, particle mean size is less than 1 μm.
5. the soft magnetic ferrite of the high magnetoconductivity low temperature degree coefficient according to any one of claim 1-4, its feature exists In its raw material is included by molar part: ferrum oxide 49.5-51.5 part, nickel oxide 17.5-18.5 part, zinc oxide 15.6-17.2 part, Manganese carbonate 2.9-3.5 part, cobalt sesquioxide 0.38-0.52 part, vanadium oxide 0.08-0.12 part, tin ash 0.02-0.04 part, Aluminium sesquioxide 0.008-0.012 part, titanium dioxide 0.045-0.055 part, Tungstic anhydride. 0.025-0.035 part, chromium oxide 0.08-0.12 part, Composite sintering agent 0.28-0.42 part;
Polyvinyl alcohol water solution and zinc stearate, the content of polyvinyl alcohol water solution accounts for the 3.5-4.5wt% of raw material total amount, Hard Fat The content of sour zinc accounts for the 0.8-1.2wt% of raw material total amount.
6. the soft magnetic ferrite of the high magnetoconductivity low temperature degree coefficient according to any one of claim 1-5, its feature exists In its raw material is included by molar part: 50.5 parts of ferrum oxide, 18.0 parts of nickel oxide, 16.4 parts of zinc oxide, 3.2 parts of manganese carbonate, three oxygen Change 0.45 part of two cobalt, 0.10 part of vanadium oxide, 0.03 part of tin ash, 0.010 part of aluminium sesquioxide, 0.05 part of titanium dioxide, three 0.03 part of tungsten oxide, 0.10 part of chromium oxide, 0.35 part of Composite sintering agent;
Polyvinyl alcohol water solution and zinc stearate, the content of polyvinyl alcohol water solution accounts for the 4wt% of raw material total amount, zinc stearate Content accounts for the 1.0wt% of raw material total amount.
7. the preparation of the soft magnetic ferrite of high magnetoconductivity low temperature degree coefficient described in a kind of any one according to claim 1-6 Method is it is characterised in that comprise the steps:
S1, mixing: ferrum oxide, nickel oxide, zinc oxide, manganese carbonate and cobalt sesquioxide are put into vibromill 1- in vibrating mill 2h, makes dispensing be sufficiently mixed and obtains material a;
S2, pre-burning: material a is carried out in pushed bat kiln pre-burning and obtain material b;
S3, pulverizing: add vanadium oxide, tin ash, aluminium sesquioxide, titanium dioxide, Tungstic anhydride. and chromium oxide in material b After carry out waterproof pulverization, be subsequently adding zinc stearate and Composite sintering agent mix homogeneously obtain material c;
S4, pelletize: add the polyvinyl alcohol water solution of the 1.6-2.2% being equivalent to material c weight in material c, using spraying Pelletize, obtains particulate material;
S5, compacting: the particulate material obtaining in s4 is obtained blank using powder former compacting;
S6, sintering: blank is put in resistance furnace and is sintered, sintering processes include: be warming up to 1200-1300 DEG C, protect Warm 10-30min, is then cooled to 1150-1180 DEG C, is incubated 2-4h, then 1280-1350 DEG C of intensification, is incubated 2-4h, then certainly So it is cooled to the soft magnetic ferrite that room temperature obtains high magnetoconductivity low temperature degree coefficient.
8. the preparation method of the soft magnetic ferrite of high magnetoconductivity low temperature degree coefficient according to claim 7, its feature It is, in s2, calcined temperature is 1000-1100 DEG C, burn-in time is 2-4h.
CN201610719250.XA 2016-08-25 2016-08-25 Soft magnetic ferrite material with high magnetic conductivity and low temperature coefficient and preparation method thereof Pending CN106348742A (en)

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