CN105924146A - Wide temperature range nickel-zinc LTCF material for high power multilayer-chip type ferrite devices and preparation method therefor - Google Patents

Wide temperature range nickel-zinc LTCF material for high power multilayer-chip type ferrite devices and preparation method therefor Download PDF

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CN105924146A
CN105924146A CN201610260375.0A CN201610260375A CN105924146A CN 105924146 A CN105924146 A CN 105924146A CN 201610260375 A CN201610260375 A CN 201610260375A CN 105924146 A CN105924146 A CN 105924146A
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ltcf
wide temperature
type ferrite
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CN105924146B (en
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刘兴
陈轲
王升
何超
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SOUTHWEST INSTITUTE OF APPLIED MAGNETICS
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—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
    • 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
    • C04B35/2666—Other ferrites containing nickel, copper or cobalt
    • C—CHEMISTRY; METALLURGY
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—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
    • 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
    • C04B35/2658—Other ferrites containing manganese or zinc, e.g. Mn-Zn ferrites
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/6261—Milling
    • C04B35/62615—High energy or reactive ball milling
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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Abstract

The invention discloses a wide temperature range nickel-zinc LTCF material for high power multilayer-chip type ferrite devices. The main constituent of the LTCF material comprises the following components in the mole percentage: 8mol% to 35mol% of nickel oxide, 9mol% to 35mol% of zinc oxide, 8mol% to 12mol% of cupric oxide and 51mol% to 58mol% of ferric oxide. The present invention also discloses the preparation method of the material. The material has an excellent microscopic structure. The compensation point which shows the position of the peak II is moved below minus 55 degrees Celsius. The ui-T curve between the peak I and peak II is relatively flat. The temperature stability of the material is good. The material meets the requirements of the operational reliability and the environmental suitability of the magnetic property of the high power multilayer-chip type ferrite devices produced by using LTCF multilayer lamination technique under the application environment of high and low temperature in the wide temperature range from minus 55 degrees Celsius to 85 degrees Celsius.

Description

High-power multilayer sheet type ferrite device wide temperature nickel zinc LTCF material and preparation method
Technical field
The present invention relates to Ferrite Material technical field, particularly relate to a kind of high-power multilayer sheet type ferrite device Part wide temperature nickel zinc LTCF material and preparation method.
Background technology
Modern military equipment, armament systems, Aeronautics and Astronautics engineering etc. to the volume of electronic system, weight and The requirement of performance is increasingly stricter, electronic building brick required for the most spaceborne, missile-borne, airborne weapon system, Parts, the direction towards little, light, thin and highly reliable, high-performance, high speed is developed especially.Currently as The switching power converters of electric supply system heart component, needs to carry out miniaturization, high reliability sets especially Meter, and power-type LTCF inductance substrate (the i.e. ferrite substrate of integrated power inductance, wherein LTCF (Low Temperature Co-fired Ferrite), the most low temperature co-fired ferrite) and chip magnetic power device (such as micro-magnetic transformer etc.), be realize element passive integration and switching power converters miniaturization, lightness, High-performance, an important means of high reliability, its key is again power-type nickel zinc LTCF material.
Conventional blocks power-type nickel-zinc-ferrite material is due to firing temperature high (more than 1100 DEG C), powder at present Material granularity is big and distribution width (D50: 3 μm～10 μm), it is not suitable for LTCF technique；And at LTCF Multi-layer stacks Technology obtains the ordinary power type nickel zinc LTCF material of through engineering approaches application, due to self Power consumption is relatively low, big electric current, high pressure by time be lost relatively low, device heating amount is little, can be used for sending out device The strictest high-current inductor of thermal control, the micro-magnetic transformer of power-type, supply convertor power ferrum oxygen The fields such as structure base board.On the premise of meeting LTCF technique, its formula design focal point is mainly reflected in the highest The crucial magnetic property index such as pcrmeability, low-power consumption, sintering temperature about 900 DEG C take into account in realization, And ignoring the wide temperature design of magnetic property, magnetism of material can (magnetic permeability μiOr inductance value L) temperature characterisitic phase Preferably temperature limit is only existed between-20～+85 DEG C, generally there is wide temperature-55～+85 DEG C high and low Temperature environment magnetic can change greatly, the problem of temperature stability difference；Cause multilayer sheet type ferrite device especially Even if being that high-power multilayer sheet type ferrite device is by adjusting device air gap area, the number of plies, sintering curre etc. Method coordinates and still suffers from high and low temperature applied environment magnetic and can change greatly, under poor stability, particularly low temperature The problem that leakage inductance is big, has a strong impact on dependability and environmental suitability (-55～+85 DEG C of electricity of device performance Sensibility reciprocal L rate of change requires as-30%～+200%).
Summary of the invention
An object of the present invention, in that a kind of high-power multilayer sheet type ferrite device wide temperature nickel is provided Zinc LTCF material, to solve the problems referred to above.
To achieve these goals, the technical solution used in the present invention is such that a kind of high-power multilayer tablet Formula ferrite device width temperature nickel zinc LTCF material, its main constituent is the following component with molar percent:
NiO 8mol%～35mol%
ZnO 9mol%～35mol%
CuO 8mol%～12mol%
Fe2O351mol%～58mol%.
As preferred technical scheme, also include the auxiliary element V of mass percent2O50.3wt%～ 0.7wt%.
As preferred technical scheme: described LTCF material is LTCF100, LTCF300 or LTCF500.
As further preferred technical scheme, the main constituent of described LTCF100 material is with molar percentage The following component of meter:
NiO 25mol%～32mol%
ZnO 9mol%～14mol%
CuO 8mol%～12mol%
Fe2O351mol%～58mol%.
Technical scheme as further preferred: the main constituent of described LTCF300 material is with molar percentage The following component of meter:
NiO 18mol%～23mol%
ZnO 16mol%～22mol%
CuO 8mol%～12mol%
Fe2O351mol%～58mol%.
Technical scheme as further preferred: the main constituent of described LTCF500 material is with molar percentage The following component of meter:
NiO 8mol%～12mol%
ZnO 26mol%～33mol%
CuO 8mol%～12mol%
Fe2O351mol%～58mol%.
The present inventor, by substantial amounts of experimentation, uses NiCuZn richness ferrum (Fe2O3Content 50mol%) it is not added with Co formula and controls Zn2+、Fe2+Content, to reduce the power attenuation of material；Meanwhile, adopt With higher Cu content formula, add appropriate low-melting-point material V2O5Reduce sintering temperature and coordinate wet method abrasive material Technique refinement powder particles (particle size distribution D50＜ 2.5 μm) method, make material burn till at about 900 DEG C After there is excellent microstructure (crystal grain is tiny, the most complete, internal porosity is few and dispersion etc.), μi—T Curve is flatter, and temperature stability is good.
The two of the purpose of the present invention, are to provide the preparation method of a kind of above-mentioned material, the technical scheme of employing For: comprise the following steps:
A. dry method batch mixing: proportionally take described main constituent, broken rear mix homogeneously, obtain compound, mixed The material time is 30～60min；
B. presintering: the compound of step A gained is carried out presintering, pre-sintering temperature is 750～850 DEG C, Obtain presintering material；
C. wet method abrasive material: by the presintering material of step B gained, add the V of described ratio2O5, carry out wet Method abrasive material, controls powder particles particle size distribution D50＜ 2.5 μm, obtains hyperfine ferrite particle；Wet grinding mill Expect and control suitable granularity, sintering temperature can be reduced.
D. double sintering: by the hyperfine ferrite particle of step C gained, carries out double sintering, sintering Temperature is 850～910 DEG C, obtains finished product.
As preferred technical scheme: step A is to use high frequency vibrating mixing system to carry out batch mixing.
Main constituent raw material oxide can be made to reach high-speed breakage effect and be effectively improved the oxidation of each raw material The being mixed evenly property of thing.
As preferred technical scheme: step B is to carry out in sintering kiln.
As preferred technical scheme: step C is to carry out in big flow recirculation system sand grinding machine.
Big flow recirculation system sand grinding machine wet method abrasive material is used to carry out powder particles refinement, to improve powder activity, fall Low reaction activation energy also effectively reduces sintering temperature, and prepared powder particles distribution is suitable to LTCF casting technique Require (conventional abrasive material D50: 3 μm～10 μm, granularity is big, distribution width, lack of homogeneity).
As preferred technical scheme: step D is to use LTCF multi-layer stacks technique to carry out.
Material is suitable to LTCF multi-layer stacks technique, and meets chip device making performance requirement.
Compared with prior art, it is an advantage of the current invention that: the wide temperature nickel zinc LTCF material of the present invention, The magnetic permeability μ of LTCF100 materiali100 ± 20%, power consumption Pv≤100kW/m3(100KHz@30mT, 20 DEG C), Sintering temperature 850～910 DEG C, magnetic permeability μiRate of change ＜ 20% (-55～+85 DEG C), LTCF300 material: Magnetic permeability μi300 ± 20%, power consumption Pv≤130kW/m3(100KHz@30mT, 20 DEG C), sintering temperature 850～ 910 DEG C, magnetic permeability μiRate of change ＜ 20% (-55～+85 DEG C), LTCF500 material: magnetic permeability μi 500 ± 20%, power consumption Pv≤150kW/m3(100KHz@30mT, 20 DEG C), sintering temperature 850～910 DEG C, Magnetic permeability μiRate of change ＜ 20% (-55～+85 DEG C)；After burning till at about 900 DEG C, there is excellent microstructure, Occurring that the compensation point of II peak has moved into less than-55 DEG C, I, II peak-to-peak has flatter μi—T Curve, temperature stability is good, meets high-power multilayer tablet under wide temperature-55～+85 DEG C of high and low temperature applied environments The dependability of formula ferrite device magnetic property and environmental suitability require that (inductance value L rate of change is -30%～+200%).
Accompanying drawing explanation
Fig. 1 is width temperature power-type LTCF material μ of the present inventioniT curve figure；
Fig. 2 is ordinary power type LTCF500 material μiT curve figure.
Fig. 3 is micro-magnetic transformer L T curve figure that width temperature LTCF material of the present invention makes；
Fig. 4 is micro-magnetic transformer L T curve that conventional LTCF500 material makes.
Detailed description of the invention
Below in conjunction with accompanying drawing, the invention will be further described.
Embodiment 1:
A kind of high-power multilayer sheet type ferrite device wide temperature nickel zinc LTCF100 material, it is main Composition is by mole meter, such as table 1:
The main constituent example (unit is molar percentage) of table 1 wide temperature LTCF100 material
NiO ZnO CuO Fe2O3
Group 1 32 9 8 51
Group 2 27 10 9 54
Group 3 25 9 8 58
Group 1, group 2 and group 3 the most also include above-mentioned main constituent gross weight 0.3%, 0.5%, 0.7% V2O5,
Preparation method is, comprises the following steps:
A. dry method batch mixing: proportionally take described main constituent, after using high frequency vibrating mixing system broken Mix homogeneously, obtains compound, and mixing time is 30min；
B. presintering: the compound of step A gained is carried out in sintering kiln presintering, in advance Sintering temperature is 850 DEG C, obtains presintering material；
C. wet method abrasive material: by the presintering material of step B gained, add the V of described ratio2O5, In big flow recirculation system sand grinding machine, carry out wet method abrasive material, control powder particles particle size distribution D50＜ 2.0 μm, obtain hyperfine ferrite particle；
D. double sintering: by the hyperfine ferrite particle of step C gained, carry out secondary burning Knot, sintering temperature is 910 DEG C, obtains finished product.
Embodiment 2:
A kind of high-power multilayer sheet type ferrite device wide temperature nickel zinc LTCF300 material, it is main Composition is by mole meter, such as table 2:
The main constituent example (unit is molar percentage) of table 2 wide temperature LTCF300 material
NiO ZnO CuO Fe2O3
Group 4 19 22 8 51
Group 5 20 18 10 52
Group 6 18 16 8 58
Group 4, group 5 and group 6 the most also include above-mentioned main constituent gross weight 0.3%, 0.4%, 0.7% V2O5,
Preparation method is, comprises the following steps:
A. dry method batch mixing: proportionally take described main constituent, after using high frequency vibrating mixing system broken Mix homogeneously, obtains compound, and mixing time is 50min；
B. presintering: the compound of step A gained is carried out in sintering kiln presintering, in advance Sintering temperature is 820 DEG C, obtains presintering material；
C. wet method abrasive material: by the presintering material of step B gained, add the V of described ratio2O5, In big flow recirculation system sand grinding machine, carry out wet method abrasive material, control powder particles particle size distribution D50＜ 2.0 μm, obtain hyperfine ferrite particle；
D. double sintering: by the hyperfine ferrite particle of step C gained, carry out secondary burning Knot, sintering temperature is 900 DEG C, obtains finished product.
Embodiment 3:
A kind of high-power multilayer sheet type ferrite device wide temperature nickel zinc LTCF500 material, it is main Composition is by mole meter, such as table 3:
The main constituent example (unit is molar percentage) of table 3 wide temperature LTCF500 material
NiO ZnO CuO Fe2O3
Group 7 12 29 8 51
Group 8 10 27 10 53
Group 9 8 26 8 58
Group 7, group 8 and group 9 the most also include above-mentioned main constituent gross weight 0.4%, 0.5%, 0.7% V2O5,
Preparation method is, comprises the following steps:
A. dry method batch mixing: proportionally take described main constituent, after using high frequency vibrating mixing system broken Mix homogeneously, obtains compound, and mixing time is 60min；
B. presintering: the compound of step A gained is carried out in sintering kiln presintering, in advance Sintering temperature is 750 DEG C, obtains presintering material；
C. wet method abrasive material: by the presintering material of step B gained, add the V of described ratio2O5, In big flow recirculation system sand grinding machine, carry out wet method abrasive material, control powder particles particle size distribution D50＜ 2.0 μm, obtain hyperfine ferrite particle；
D. double sintering: by the hyperfine ferrite particle of step C gained, carry out secondary burning Knot, sintering temperature is 900 DEG C, obtains finished product.
Embodiment 4
Material properties test
It is respectively adopted group 8 institute of the group 2 of embodiment 1, the group 5 of embodiment 2 and embodiment 3 The product obtained, is measured μiT curve (test condition is 100mV, 10KHz) and micro- (test condition is 500mV, 100KHz to magnetic transformer L T curve, transformator model 10 × 10 × 3 (mm)), its result is as shown in figures 1 and 3.
Comparative example: use ordinary power type nickel zinc LTCF500 material, its main constituent is by moles hundred Proportion by subtraction meter, such as table 4:
The main constituent example (unit is molar percentage) of the conventional LTCF500 material of table 4
NiO ZnO CuO Co2O3 Fe2O3
Group 10 12 33 10.78 0.22 44
Group 11 11 29 11.82 0.18 48
Group 12 13 27 10.84 0.16 49
Group 10, group 11 and group 12 the most also include above-mentioned main constituent gross weight 0.4%, 0.5%, The V of 0.7%2O5,
Preparation method is, comprises the following steps:
A. dry method batch mixing: proportionally take described main constituent, after using high frequency vibrating mixing system broken Mix homogeneously, obtains compound, and mixing time is 60min；
B. presintering: the compound of step A gained is carried out in sintering kiln presintering, in advance Sintering temperature is 780 DEG C, obtains presintering material；
C. wet method abrasive material: by the presintering material of step B gained, add the V of described ratio2O5, In big flow recirculation system sand grinding machine, carry out wet method abrasive material, control powder particles particle size distribution D50＜ 2.0 μm, obtain hyperfine ferrite particle；
D. double sintering: by the hyperfine ferrite particle of step C gained, carry out secondary burning Knot, sintering temperature is 900 DEG C, obtains finished product.
Use the product of comparative example group 11 gained, carry out under the same conditions as above testing material Material μiT curve (test condition is 100mV, 10KHz) and micro-magnetic transformer L T curve (test condition is 500mV, 100KHz, transformator model 10 × 10 × 3 (mm)), its knot Fruit is as shown in Figure 2 and Figure 4.
From Fig. 1-4 it can be seen that
1.μiT curve:
Ordinary power type nickel zinc LTCF500 material uses NiCuZn to owe ferrum (Fe2O3Content ＜ 50mol%) add Co formula to make, go out the temperature position of item II peak compensation point at about-20 DEG C, μ below this temperatureiT changes the most greatly；μiT curve is at-20 DEG C～+85 DEG C I, II peak Between bigger trench occurs, temperature stability is poor；
And the material of the present invention, go out the temperature position of item II peak compensation point have moved into-55 DEG C with Under, μiT curve has a flatter region, the temperature of pcrmeability between-55 DEG C～+85 DEG C Stability and environmental suitability are preferable.
The most micro-magnetic transformer L T curve:
Micro-magnetic transformer change of L T curve between-55 DEG C～+85 DEG C that conventional material makes Rule and material μiT curve change is similar, and the temperature stability of inductance value L and environment adapt to Property the most poor, in especially less than-20 DEG C low temperature environments leakage inductance loss bigger；
And micro-magnetic transformer L T curve between-55 DEG C～+85 DEG C that the material of the present invention makes Changing Pattern and material μiT curve change is similar, the temperature stability of inductance value L and ring Border adaptability is all preferable, and between especially-20 DEG C～-55 DEG C, the leakage inductance in low temperature environment is lost very Little.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, All any amendment, equivalent and improvement etc. made within the spirit and principles in the present invention, Should be included within the scope of the present invention.

Claims (10)

1. a high-power multilayer sheet type ferrite device wide temperature nickel zinc LTCF material, it is characterised in that its main constituent is the following component with molar percent:
NiO 8mol%～35mol%
ZnO 9mol%～35mol%
CuO 8mol%～12mol%
Fe2O3 51mol%～58mol%.
High-power multilayer sheet type ferrite device the most according to claim 1 wide temperature nickel zinc LTCF material, it is characterised in that also include the auxiliary element V of mass percent2O5 0.3wt%～0.7wt%.
High-power multilayer sheet type ferrite device the most according to claim 1 wide temperature nickel zinc LTCF material, it is characterised in that: described LTCF material is LTCF100, LTCF300 or LTCF500.
High-power multilayer sheet type ferrite device the most according to claim 3 wide temperature nickel zinc LTCF material, it is characterised in that the main constituent of described LTCF100 material is the following component with molar percent:
NiO 25mol%～32mol%
ZnO 9mol%～14mol%
CuO 8mol%～12mol%
Fe2O3 51mol%～58mol%.
High-power multilayer sheet type ferrite device the most according to claim 3 wide temperature nickel zinc LTCF material, it is characterised in that the main constituent of described LTCF300 material is the following component with molar percent:
NiO 18mol%～23mol%
ZnO 16mol%～22mol%
CuO 8mol%～12mol%
Fe2O3 51mol%～58mol%.
High-power multilayer sheet type ferrite device the most according to claim 3 wide temperature nickel zinc LTCF material, it is characterised in that the main constituent of described LTCF500 material is the following component with molar percent:
NiO 8mol%～12mol%
ZnO 26mol%～33mol%
CuO 8mol%～12mol%
Fe2O3 51mol%～58mol%.
7. the preparation method of the high-power multilayer sheet type ferrite device wide temperature nickel zinc LTCF material described in claim 2, it is characterised in that comprise the following steps:
A. dry method batch mixing: proportionally take described main constituent, broken rear mix homogeneously, obtain compound, mixing time is 30～60min；
B. presintering: the compound of step A gained is carried out presintering, and pre-sintering temperature is 750～850 DEG C, obtains presintering material；
C. wet method abrasive material: by the presintering material of step B gained, add the V of described ratio2O5, carry out wet method abrasive material, control powder particles particle size distributionD 50 ＜ 2.5 μm, obtains hyperfine ferrite particle；
D. double sintering: by the hyperfine ferrite particle of step C gained, carrying out double sintering, sintering temperature is 850～910 DEG C, obtains finished product.
Method the most according to claim 7, it is characterised in that: step A is to use high frequency vibrating mixing system to carry out batch mixing, and step B is to carry out in sintering kiln.
Method the most according to claim 7, it is characterised in that: step C is to carry out in big flow recirculation system sand grinding machine.
Method the most according to claim 7, it is characterised in that: step D is to use LTCF multi-layer stacks technique.
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Citations (4)

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