CN105924146B - High-power multilayer sheet type ferrite device wide warm nickel zinc LTCF materials and preparation method - Google Patents

High-power multilayer sheet type ferrite device wide warm nickel zinc LTCF materials and preparation method Download PDF

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CN105924146B
CN105924146B CN201610260375.0A CN201610260375A CN105924146B CN 105924146 B CN105924146 B CN 105924146B CN 201610260375 A CN201610260375 A CN 201610260375A CN 105924146 B CN105924146 B CN 105924146B
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ltcf
multilayer sheet
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sintering
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CN105924146A (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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    • 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
    • C04B35/2666—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
    • C04B2235/3239—Vanadium oxides, vanadates or oxide forming salts thereof, e.g. magnesium vanadate
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
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Abstract

The invention discloses a kind of high-power multilayer sheet type ferrite device warm nickel zinc LTCF materials of width, its principal component is the following component with molar percent：NiO 8mol%~35mol%, ZnO 9mol%~35mol%, CuO 8mol%~12mol%, Fe2O3 51mol%~58mol%, the invention also discloses the preparation method of the material, material of the invention has excellent microstructure, and the compensation point for II peak position occur has moved into less than 55 DEG C, and I, II is peak-to-peak with flatterμ i - T curve, temperature stability is good, meets use reliability and the environmental suitability requirement that the high-power multilayer sheet type ferrite device magnetic property of LTCF multi-layer stacks technique making is used under wide 55~+85 DEG C of high and low temperature application environments of temperature.

Description

High-power multilayer sheet type ferrite device wide warm nickel zinc LTCF materials and preparation method
Technical field
The present invention relates to Ferrite Material technical field, more particularly to a kind of high-power multilayer sheet type ferrite device are wide Warm nickel zinc LTCF materials and preparation method.
Background technology
Modern military equipment, weapon system, Aeronautics and Astronautics engineering etc. will to the volume of electronic system, weight and performance Ask increasingly stringenter, particularly spaceborne, missile-borne, the required electronic building brick of airborne weapon system, component, even more towards it is small, light, Thin and highly reliable, high-performance, the direction of high speed are developed.Converted currently as the Switching Power Supply of electric supply system heart component Device, even more needs to be minimized, High Reliability Design, and power-type LTCF inductance substrates (the i.e. iron oxygen of integrated power inductance Structure base board, wherein LTCF (Low Temperature Co-fired Ferrite), i.e., low temperature co-fired ferrite) and chip magnetism Power device (such as micro- magnetic transformer), is to realize element passive integration and switching power converters miniaturization, lightness, Gao Xing Energy, an important means of high reliability, it is crucial and is power-type nickel zinc LTCF materials.
At present conventional blocks power-type nickel-zinc-ferrite material due to firing temperature high (being more than 1100 DEG C), powder particles it is big And wide (the D of distribution50：3 μm~10 μm), it is not suitable for LTCF techniques；And obtain work in LTCF multi-layer stacks technologies Journeyization application ordinary power type nickel zinc LTCF materials, since oneself power consumption is relatively low, high current, high pressure by when loss compared with Low, device heating amount is small, available for device heating is controlled more stringent high-current inductor, the micro- magnetic transformer of power-type, The supply convertor fields such as power ferrite substrate.It is formulated design focal point major embodiment on the premise of LTCF techniques are met In taking into account in realization beneficial to the crucial magnetic property index such as high magnetic permeability, low-power consumption, 900 DEG C or so of sintering temperature, and neglect Depending on the width temperature design of magnetic property, magnetism of material can (magnetic permeability μiOr inductance value L) temperature characterisitic preferably applies temperature relatively Between scope only exists in -20~+85 DEG C, wide temperature -55~+85 DEG C high and low temperature environment magnetic of generally existing can change greatly, and temperature is steady The problem of qualitative difference；Even if cause the especially high-power multilayer sheet type ferrite device of multilayer sheet type ferrite device by adjusting The cooperation of the methods of device air gap area, the number of plies, sintering curre, which still suffers from high and low temperature application environment magnetic, can change big, stabilization Property it is poor, particularly leakage inductance is big under low temperature the problem of, seriously affect device performance use reliability and environmental suitability (- 55~+ 85 DEG C of inductance value L change rates requirements are -30%~+200%).
The content of the invention
An object of the present invention, in that provide a kind of high-power multilayer sheet type ferrite device with wide warm nickel zinc LTCF Material, to solve the above problems.
To achieve these goals, the technical solution adopted by the present invention is such：A kind of high-power multilayer sheet type iron oxygen The wide warm nickel zinc LTCF materials of body device, its principal component is the following component with molar percent：
NiO 8mol%~35mol%
ZnO 9mol%~35mol%
CuO 8mol%~12mol%
Fe2O351mol%~58mol%.
As preferable technical solution, the auxiliary element V of mass percent meter is further included2O50.3wt%~0.7wt%.
As preferable technical solution：The LTCF materials are LTCF100, LTCF300 or LTCF500.
As further preferred technical solution, the principal components of the LTCF100 materials be with molar percent as Lower component：
NiO 25mol%~32mol%
ZnO 9mol%~14mol%
CuO 8mol%~12mol%
Fe2O351mol%~58mol%.
As further preferred technical solution：The principal component of the LTCF300 materials be with molar percent as Lower component：
NiO 18mol%~23mol%
ZnO 16mol%~22mol%
CuO 8mol%~12mol%
Fe2O351mol%~58mol%.
As further preferred technical solution：The principal component of the LTCF500 materials be with molar percent as Lower component：
NiO 8mol%~12mol%
ZnO 26mol%~33mol%
CuO 8mol%~12mol%
Fe2O351mol%~58mol%.
The present inventor is by substantial amounts of experimental study, using NiCuZn richness iron (Fe2O3Content ﹥ 50mol%) it is not added with Co is formulated and controls Zn2+、Fe2+Content, to reduce the power attenuation of material；Meanwhile the higher Cu contents formula of use, addition Appropriate low-melting-point material V2O5Reduce sintering temperature and coordinate wet method abrasive material technique refinement powder particles (size distribution D502.5 μm of ＜) Method, make material have after being burnt till at 900 DEG C or so excellent microstructure (crystal grain is tiny, uniformly complete, internal porosity it is few and Disperse), μi- T curve is flatter, and temperature stability is good.
The second object of the present invention is to provide a kind of preparation method of above-mentioned material, the technical solution used for：Including Following steps：
A. dry method batch mixing：The principal component is proportionally taken, is uniformly mixed after crushing, obtains mixture, mixing time is 30~60min；
B. it is pre-sintered：Mixture obtained by step A is subjected to pre-sintering, pre-sintering temperature is 750~850 DEG C, is obtained pre- Sintering feed；
C. wet method abrasive material：By in the presintering material obtained by step B, the V of the ratio is added2O5, carry out wet method abrasive material, control Powder particles size distribution D processed502.5 μm of ＜, obtains hyperfine ferrite particle；Wet method abrasive material simultaneously controls suitable granularity, can To reduce sintering temperature.
D. double sintering：Hyperfine ferrite particle obtained by by step C, carries out double sintering, sintering temperature for 850~ 910 DEG C, obtain finished product.
As preferable technical solution：Step A is to carry out batch mixing using high frequency vibrating mixing system.
Principal component raw material oxide can be made to reach high-speed breakage effect and effectively improve the mixed of each raw material oxide And uniformity.
As preferable technical solution：Step B is carried out in sintering kiln.
As preferable technical solution：Step C is carried out in big flow circulates sand mill.
Powder particles refinement is carried out using big flow circulation sand mill wet grinding mill material, to improve powder activity, reduce and react Activation and can effectively reduce sintering temperature, and obtained powder particles distribution is suitable for LTCF casting techniques and requires (conventional abrasive material D50：3μ M~10 μm, granularity is big, distribution is wide, lack of homogeneity).
As preferable technical solution：Step D is carried out using LTCF multi-layer stacks technique.
Material is suitable for LTCF multi-layer stacks techniques, and meets that chip device makes performance requirement.
Compared with prior art, the advantage of the invention is that：The warm nickel zinc LTCF materials of width of the present invention, LTCF100 materials Magnetic permeability μi100 ± 20%, power consumption Pv≤100kW/m3(100KHz@30mT, 20 DEG C), 850~910 DEG C of sintering temperature, magnetic conductance Rate μiChange rate ＜ 20% (- 55~+85 DEG C), LTCF300 materials：Magnetic permeability μi300 ± 20%, power consumption Pv≤130kW/m3 (100KHz@30mT, 20 DEG C), 850~910 DEG C of sintering temperature, magnetic permeability μiChange rate ＜ 20% (- 55~+85 DEG C), LTCF500 materials：Magnetic permeability μi500 ± 20%, power consumption Pv≤150kW/m3(100KHz@30mT, 20 DEG C), sintering temperature 850~ 910 DEG C, magnetic permeability μiChange rate ＜ 20% (- 55~+85 DEG C)；There is excellent microstructure after being burnt till at 900 DEG C or so, occur The compensation point of II peak position has moved into less than -55 DEG C, and I, II peak-to-peak has flatter μi- T curve, temperature stability is good, Meet the use reliability of high-power multilayer sheet type ferrite device magnetic property under wide temperature -55~+85 DEG C high and low temperature application environment With environmental suitability requirement (inductance value L change rates are -30%~+200%).
Brief description of the drawings
Fig. 1 is the wide warm power-type LTCF materials μ of the present inventioni- T curve figure；
Fig. 2 is ordinary power type LTCF500 materials μi- T curve figure.
Fig. 3 is micro- magnetic transformer L-T curve figure that present invention width temperature LTCF materials make；
Fig. 4 is micro- magnetic transformer L-T curve that routine LTCF500 materials make.
Embodiment
The present invention will be further described with reference to the accompanying drawings.
Embodiment 1：
A kind of high-power multilayer sheet type ferrite device presses Mole percent with wide warm nickel zinc LTCF100 materials, its principal component Than meter, such as table 1：
The principal component example of the wide temperature LTCF100 materials of table 1 (unit is molar percentage)
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 further include the V of above-mentioned principal component gross weight 0.3%, 0.5%, 0.7% respectively2O5,
Preparation method is to comprise the following steps：
A. dry method batch mixing：The principal component is proportionally taken, is uniformly mixed, is mixed after being crushed using high frequency vibrating mixing system Close material, mixing time 30min；
B. it is pre-sintered：Mixture obtained by step A is carried out to pre-sintering in sintering kiln, pre-sintering temperature is 850 DEG C, Obtain presintering material；
C. wet method abrasive material：By in the presintering material obtained by step B, the V of the ratio is added2O5, circulate and be sanded in big flow Wet method abrasive material, control powder particles size distribution D are carried out in machine502.0 μm of ＜, obtains hyperfine ferrite particle；
D. double sintering：Hyperfine ferrite particle obtained by by step C, carries out double sintering, sintering temperature 910 DEG C, obtain finished product.
Embodiment 2：
A kind of high-power multilayer sheet type ferrite device presses Mole percent with wide warm nickel zinc LTCF300 materials, its principal component Than meter, such as table 2：
The principal component example of the wide temperature LTCF300 materials of table 2 (unit is molar percentage)
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 further include the V of above-mentioned principal component gross weight 0.3%, 0.4%, 0.7% respectively2O5,
Preparation method is to comprise the following steps：
A. dry method batch mixing：The principal component is proportionally taken, is uniformly mixed, is mixed after being crushed using high frequency vibrating mixing system Close material, mixing time 50min；
B. it is pre-sintered：Mixture obtained by step A is carried out to pre-sintering in sintering kiln, pre-sintering temperature is 820 DEG C, Obtain presintering material；
C. wet method abrasive material：By in the presintering material obtained by step B, the V of the ratio is added2O5, circulate and be sanded in big flow Wet method abrasive material, control powder particles size distribution D are carried out in machine502.0 μm of ＜, obtains hyperfine ferrite particle；
D. double sintering：Hyperfine ferrite particle obtained by by step C, carries out double sintering, sintering temperature 900 DEG C, obtain finished product.
Embodiment 3：
A kind of high-power multilayer sheet type ferrite device presses Mole percent with wide warm nickel zinc LTCF500 materials, its principal component Than meter, such as table 3：
The principal component example of the wide temperature LTCF500 materials of table 3 (unit is molar percentage)
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 further include the V of above-mentioned principal component gross weight 0.4%, 0.5%, 0.7% respectively2O5,
Preparation method is to comprise the following steps：
A. dry method batch mixing：The principal component is proportionally taken, is uniformly mixed, is mixed after being crushed using high frequency vibrating mixing system Close material, mixing time 60min；
B. it is pre-sintered：Mixture obtained by step A is carried out to pre-sintering in sintering kiln, pre-sintering temperature is 750 DEG C, Obtain presintering material；
C. wet method abrasive material：By in the presintering material obtained by step B, the V of the ratio is added2O5, circulate and be sanded in big flow Wet method abrasive material, control powder particles size distribution D are carried out in machine502.0 μm of ＜, obtains hyperfine ferrite particle；
D. double sintering：Hyperfine ferrite particle obtained by by step C, carries out double sintering, sintering temperature 900 DEG C, obtain finished product.
Embodiment 4
Material properties test
8 resulting product of group of the group 2 of embodiment 1, the group 5 of embodiment 2 and embodiment 3 is respectively adopted, is measured μi- T curve (test condition 100mV, 10KHz) and micro- magnetic transformer L-T curve (test condition 500mV, 100KHz, Transformer model 10 × 10 × 3 (mm)), its result is as shown in figures 1 and 3.
Comparative example：Using ordinary power type nickel zinc LTCF500 materials, its principal component is by mole meter, such as table 4：
The principal component example of the routine LTCF500 materials of table 4 (unit is molar percentage)
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 further include the V of above-mentioned principal component gross weight 0.4%, 0.5%, 0.7% respectively2O5,
Preparation method is to comprise the following steps：
A. dry method batch mixing：The principal component is proportionally taken, is uniformly mixed, is mixed after being crushed using high frequency vibrating mixing system Close material, mixing time 60min；
B. it is pre-sintered：Mixture obtained by step A is carried out to pre-sintering in sintering kiln, pre-sintering temperature is 780 DEG C, Obtain presintering material；
C. wet method abrasive material：By in the presintering material obtained by step B, the V of the ratio is added2O5, circulate and be sanded in big flow Wet method abrasive material, control powder particles size distribution D are carried out in machine502.0 μm of ＜, obtains hyperfine ferrite particle；
D. double sintering：Hyperfine ferrite particle obtained by by step C, carries out double sintering, sintering temperature 900 DEG C, obtain finished product.
Using 11 resulting product of comparative example group, test material μ is carried out under the same conditions as abovei(the test of-T curve Condition is 100mV, 10KHz) and micro- magnetic transformer L-T curve (test condition 500mV, 100KHz, transformer model 10 × 10 × 3 (mm)), its result is as shown in Figure 2 and Figure 4.
It can be seen that from Fig. 1-4：
1.μi- T curve：
Ordinary power type nickel zinc LTCF500 materials owe iron (Fe using NiCuZn2O3Content ＜ 50mol%) plus Co formula systems Make, go out the temperature position of 1 peak compensation point of item at -20 DEG C or so, the μ below the temperaturei- T changes very greatly；μi- T curve - 20 DEG C~+85 DEG C I, II it is peak-to-peak there is larger trench, temperature stability is poor；
And the material of the present invention, the temperature position for going out 1 peak compensation point of item have moved into less than -55 DEG C, μi- T curve- There is a flatter region, the temperature stability and environmental suitability of magnetic conductivity are preferable between 55 DEG C~+85 DEG C.
2. micro- magnetic transformer L-T curve：
Micro- magnetic transformer that conventional material the makes changing rule of L-T curve and material μ between -55 DEG C~+85 DEG Ci—T Curvilinear motion is similar, and the temperature stability and environmental suitability of inductance value L is poor, in especially less than -20 DEG C low temperature environments Leakage inductance loss is larger；
And the changing rule and material for micro- magnetic transformer L-T curve between -55 DEG C~+85 DEG C that the material of the present invention makes Expect μiThe change of-T curve is similar, and the temperature stability and environmental suitability of inductance value L is preferable, especially -20 DEG C~-55 DEG C Between leakage inductance loss very little in low temperature environment.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention All any modification, equivalent and improvement made within refreshing and principle etc., should all be included in the protection scope of the present invention.

Claims (8)

  1. A kind of 1. wide warm nickel zinc LTCF materials of high-power multilayer sheet type ferrite device, it is characterised in that its principal component be with The following component of molar percent：
    NiO 8mol%~35mol%
    ZnO 9mol%~35mol%
    CuO 8mol%~12mol%
    Fe2O3 51mol%~58mol%；
    Further include the auxiliary element V of mass percent meter2O5 0.3wt%~0.7wt%；
    The preparation method of above-mentioned material.Comprise the following steps：
    A. dry method batch mixing：Proportionally take the principal component, be uniformly mixed after crushing, obtain mixture, mixing time for 30~ 60min；
    B. it is pre-sintered：Mixture obtained by step A is subjected to pre-sintering, pre-sintering temperature is 750~850 DEG C, obtains pre-sintering Material；
    C. wet method abrasive material：By in the presintering material obtained by step B, the V of the ratio is added2O5, wet method abrasive material is carried out, controls powder Expect particle size distribution D502.5 μm of ＜, obtains hyperfine ferrite particle；
    D. double sintering：Hyperfine ferrite particle obtained by by step C, carries out double sintering, and sintering temperature is 850~910 DEG C, obtain finished product.
  2. 2. high-power multilayer sheet type ferrite device according to claim 1 is existed with wide warm nickel zinc LTCF materials, its feature In：The LTCF materials are LTCF100, LTCF300 or LTCF500.
  3. 3. high-power multilayer sheet type ferrite device according to claim 2 is existed with wide warm nickel zinc LTCF materials, its feature In the principal component of the LTCF100 materials is the following component with molar percent：
    NiO 25mol%~32mol%
    ZnO 9mol%~14mol%
    CuO 8mol%~12mol%
    Fe2O3 51mol%~58mol%.
  4. 4. high-power multilayer sheet type ferrite device according to claim 2 is existed with wide warm nickel zinc LTCF materials, its feature In the principal component of the LTCF300 materials is the following component with molar percent：
    NiO 18mol%~23mol%
    ZnO 16mol%~22mol%
    CuO 8mol%~12mol%
    Fe2O3 51mol%~58mol%.
  5. 5. high-power multilayer sheet type ferrite device according to claim 2 is existed with wide warm nickel zinc LTCF materials, its feature In the principal component of the LTCF500 materials is the following component with molar percent：
    NiO 8mol%~12mol%
    ZnO 26mol%~33mol%
    CuO 8mol%~12mol%
    Fe2O3 51mol%~58mol%.
  6. 6. according to the method described in claim 1, it is characterized in that：Step A is to carry out batch mixing, step using high frequency vibrating mixing system B is carried out in sintering kiln.
  7. 7. according to the method described in claim 1, it is characterized in that：Step C is carried out in big flow circulates sand mill.
  8. 8. according to the method described in claim 1, it is characterized in that：Step D is to use LTCF multi-layer stacks techniques.
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