CN102050622A - Low-temperature sintering soft magnetic ferrite material, magnesium, copper and zinc ferrite and preparation methods thereof - Google Patents

Low-temperature sintering soft magnetic ferrite material, magnesium, copper and zinc ferrite and preparation methods thereof Download PDF

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CN102050622A
CN102050622A CN 201010551863 CN201010551863A CN102050622A CN 102050622 A CN102050622 A CN 102050622A CN 201010551863 CN201010551863 CN 201010551863 CN 201010551863 A CN201010551863 A CN 201010551863A CN 102050622 A CN102050622 A CN 102050622A
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soft magnetic
low
temperature sintering
magnesium
ferrite
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陈鲁国
朱建华
李建辉
樊应县
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Shenzhen Zhenhua Ferrite and Ceramic Electronics Co Ltd
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Shenzhen Zhenhua Ferrite and Ceramic Electronics Co Ltd
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Abstract

The invention discloses a low-temperature sintering soft magnetic ferrite material which comprises a main material of a magnesium, copper and zinc ferrite and auxiliary materials of bismuth oxide and cobalt oxide, wherein the main material accounts for 95-99 percent by mass in the formulation, and the auxiliary materials account for 1-5 percent by mass in the formulation. Compared with the traditional soft magnetic Mg-Zn ferrite material, the low-temperature sintering soft magnetic ferrite material has greatly reduced sintering temperature reaching about 900 DEG C and can be co-fired with silver. A Ni-containing material is not used in the invention, thus the cost is greatly lowered.

Description

Low-temperature sintering soft magnetic ferrite and magnesium copper zinc ferrite and preparation method thereof
Technical field
The present invention relates to a kind of low-temperature sintering soft magnetic ferrite and a kind of magnesium copper zinc ferrite and above-mentioned two kinds of preparation methods.
Background technology
Laminated inductive/magnetic bead is a kind of important surface mount device that development in recent years is got up, and is one of indispensable slice component of surface mounting technique of new generation, is widely used in communication, computer and fields such as peripheral product and household electrical appliance thereof.
The gordian technique of preparation slice component is that magnetic media material and internal conductor material (being generally Ag) are burnt altogether.This has lower sintering temperature with regard to requiring soft magnetic ferrite wherein, has high magnetic permeability and high quality factor simultaneously.Domestic and international general inductive material mainly concentrates on low-temperature sintering Ni-Cu-Zn based ferrite at present, but this material is because magnetostriction coefficient is big, thereby counter stress is relatively responsive, and the stress when installing from the stress of inner wire and substrate etc. will cause the magnetism of material can variation.And the Mg-Cu-Zn Ferrite Material has lower magnetostriction coefficient, and good magnetic performance and sintering characteristic are a kind of very ideal multilayer chip inductor materials.Simultaneously, constantly go up significantly (nickel oxide accounts for more than 70% of raw materials cost) along with the nickel oxide price, and reason such as domestic manufacturer's nickel oxide performance of producing is stable inadequately, replacing nickel-zinc ferrite with MgZn ferrite is a research direction with open prospect, it not only can reduce the production cost of material greatly, and can guarantee the stability of product performance.
Chinese patent application number is in the application for a patent for invention of " 200410093230.3 " " soft magnetic Mg-Zn ferrite material and low temperature sintering technology thereof " by name, a kind of soft magnetic Mg-Zn ferrite material and low temperature sintering technology thereof are disclosed, described Mg-Zn soft magnetic ferrite is by Fe2O3, MgO, ZnO, Mn 3O 4, CuO forms, each composition and consumption thereof are as follows:
Fe 2O 3 47.5～48.7wt％
MgO 25.5～30.0wt％
ZnO 18.0～21.4wt％
Mn 3O 4 0.5～1.2wt％
Flux 3.0～4.2wt%, flux are CuO and Bi 2O 3
Auxiliary material 0～5wt%
Form with the above-mentioned raw materials low-temperature sintering, this invention has reduced sintering temperature, makes originally and is reduced to 1220 ℃ from 1320 ℃.But still can't reach the common burning temperature of silver.
At present, mainly be to be raw material both at home and abroad with magnesium oxide about the research of MgZn ferrite aspect.
Summary of the invention
The technical problem that the present invention mainly solves provides a kind of low-temperature sintering soft magnetic ferrite of low-cost and high-performance.
The present invention also provides a kind of preparation method of low-temperature sintering soft magnetic ferrite of low-cost and high-performance.
The present invention also provides a kind of magnesium copper zinc ferrite that is used to prepare the low-temperature sintering soft magnetic ferrite of low-cost and high-performance.
The present invention further provides a kind of preparation method of magnesium copper zinc ferrite of the low-temperature sintering soft magnetic ferrite that is used to prepare low-cost and high-performance.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: a kind of low-temperature sintering soft magnetic ferrite is provided, the major ingredient of described low-temperature sintering soft magnetic ferrite is the magnesium copper zinc ferrite, and the auxiliary material of described low-temperature sintering soft magnetic ferrite is bismuth oxide and cobalt oxide; Major ingredient shared mass percent in prescription is 95～99%, and auxiliary material shared mass percent in prescription is 1～5%.
The present invention can reduce greatly with respect to its sintering temperature of existing soft magnetic Mg-Zn ferrite material, reaches about 900 ℃, can burn altogether with silver.The present invention need not simultaneously to use and contains the Ni material, and cost reduces greatly.
Wherein, described magnesium copper zinc ferrite, each component can adopt following molar percentage:
Fe 2O 3： 47％～50％；
Magnesium basic carbonate in MgO: 7%～37%;
ZnO： 4％～31％；
CuO： 6％～14％。
The present invention also provides the preparation method of the low-temperature sintering soft magnetic ferrite of above-mentioned low-cost and high-performance, may further comprise the steps:
1) takes by weighing Fe 2O 3, ZnO, CuO and magnesium basic carbonate;
2), the gained slurry in 120～150 ℃ of oven dry down, is crossed 200 mesh sieves with step 1) products therefrom and deionized water mixed grinding form slurry;
3) with step 2) the back gained powder that sieves places sintering oven in 800～875 ℃ of following pre-burnings, is incubated 2～4 hours;
4) the pre-burning product with the step 3) gained mixes by prescription with bismuth oxide and cobalt oxide, and mix products and deionized water are ground to form slurry, and the gained slurry in 120～150 ℃ of oven dry down, is crossed 200 mesh sieves;
5) step 4) is sieved back gained powder adds tackiness agent PVA and granulation, compression moulding;
6) with the product of step 5) compression moulding at 860～950 ℃ of following sintering 4～6h.
The present invention adopts magnesium basic carbonate as the ferritic initial feed of low-temperature sintering MgCuZn, has obtained the magnetic permeability that shrinks behavior and can compare with it with the same sintering of NiCuZn ferrite and higher quality factor.
Among the preparation method of above-mentioned low-temperature sintering soft magnetic ferrite, step 2) or 4) described grinding can select: raw material that will be to be ground mixes back ball milling 2～3h in planetary ball mill with deionized water and zirconium post.
Among the preparation method of above-mentioned low-temperature sintering soft magnetic ferrite, the technical parameter of the described compression moulding of step 5) can be selected, and forming pressure is 6MPa, pressurize 10～15s.
The present invention also provides a kind of magnesium copper zinc ferrite, described magnesium copper zinc ferrite, and the molar percentage of each component is as follows:
Fe 2O 3： 47％～50％；
Magnesium basic carbonate in MgO: 7%～37%;
ZnO： 4％～31％；
CuO： 6％～14％。
Above-mentioned materials can be used to prepare the low-temperature sintering soft magnetic ferrite of low-cost and high-performance.
The preparation method of above-mentioned magnesium copper zinc ferrite may further comprise the steps:
1) gets Fe by stoichiometric ratio 2O 3, ZnO, CuO and magnesium basic carbonate;
2), the gained slurry in 120～150 ℃ of oven dry down, is crossed 200 mesh sieves with step 1) products therefrom and deionized water mixed grinding form slurry;
3) with step 2) the back gained powder that sieves places sintering oven in 800～875 ℃ of following pre-burnings, is incubated 2～4 hours.
The present invention adopts magnesium basic carbonate as the ferritic initial feed of low-temperature sintering MgCuZn, and products obtained therefrom can be used for preparing the low-temperature sintering soft magnetic ferrite of low-cost and high-performance.
Wherein, step 2) described grinding is: raw material that will be to be ground mixes back ball milling 2～3h in planetary ball mill with deionized water and zirconium post.
Embodiment
By describing technology contents of the present invention in detail, realized purpose and effect, give explanation below in conjunction with embodiment is detailed.
Embodiment 1
Initial feed is Fe 2O 3, magnesium basic carbonate, ZnO, CuO, take by weighing by the molar percentage of each component in the table 1, dry after adding the deionized water ball milling, 800 ℃ of following pre-burnings, be incubated 2 hours.Take by weighing the pre-imitation frosted glass of 60g, add Bi 2O 3And Co 2O 3(Bi 2O 3And Co 2O 3Weight and account for the prescription gross weight 1～5%), dry after adding water for ball milling, sieve, granulation, moulding, at 890 ℃ of following sintering, be incubated 4 hours.The external diameter 36mm of the annular sample of compression moulding, internal diameter 22mm, thickness 7～8mm, magnet ring is measured its size with digital display calliper behind the sintering, calculates shrinking percentage; Behind even coiling 20 circles of copper cash with line footpath 0.3mm, with TH2828LCR tester (1K～1MHz) inductance measuring and Q value; Utilize Archimedes's drainage bulk density, the performance perameter of the sample that obtains sees Table 1.
Figure BDA0000033251180000051
Table 1
As can be seen from Table 1, (1) μ iIncrease with Zn content increases, but high Q value district moves to low frequency simultaneously; (2) along with Cu content in the MgCuZn ferrite increases, the μ of material under the low frequency iIncrease, this is because the adulterated increase of Cu has caused the increase of grain-size, thereby has aggravated due to the domain wall displacement; (3) along with the increase of Cu content, sample rate increases gradually, and this may also be to cause μ iAnother reason that increases.
Embodiment 2
Initial feed is Fe 2O 3, magnesium basic carbonate, ZnO, CuO, Fe in molar ratio 2O 3: MgO: ZnO: CuO=48: take by weighing at 26: 16: 10, dry after adding the deionized water ball milling,, be incubated 2 hours, take by weighing the pre-imitation frosted glass of 60g, add the Bi of different deals 800 ℃ of pre-burnings 2O 3And Co 2O 3, dry after adding water for ball milling, sieve, granulation, moulding, at 890 ℃ of following sintering, be incubated 4 hours.The external diameter 36mm of the annular sample of compression moulding, internal diameter 22mm, thickness 7～8mm, magnet ring is measured its size with digital display calliper behind the sintering, calculates shrinking percentage; Behind even coiling 20 circles of copper cash with line footpath 0.3mm, with TH2828LCR tester (1K～1MHz) inductance measuring and Q value; Utilize Archimedes's drainage bulk density, the performance perameter of the sample that obtains sees Table 2.
Table 2
As can be seen from Table 2, (1) introduces a small amount of sintering agent Bi when the MgCuZn ferrite 2O 3The time, sample is densification more, simultaneously, because Bi 2O 3Existence, promoted the increase of crystal grain and the minimizing of pore, these all help moving of domain wall, thereby impel the magnetic permeability of material to increase; But work as Bi 2O 3When content further increased, magnetic permeability presented downward trend, and this may be relevant with the unusual increase of crystal grain; (2) Co 2O 3Adding make μ iReduce, but the Q value increases substantially, and high Q value is shifted to front end.
Embodiment 3
Initial feed is Fe 2O 3, magnesium basic carbonate, ZnO, CuO, Fe in molar ratio 2O 3: MgO: ZnO: CuO=48: take by weighing at 26: 16: 10, dry after adding the deionized water ball milling, 800 ℃, 875 ℃ following pre-burnings, each is incubated 2 hours.Take by weighing the pre-imitation frosted glass of 60g, add the Bi of 3wt% 2O 3Co with 0.2wt% 2O 3, dry after adding water for ball milling, sieve, granulation, moulding, at 890 ℃, 910 ℃ following sintering, be incubated 4 hours.The external diameter 36mm of the annular sample of compression moulding, internal diameter 22mm, thickness 7～8mm, magnet ring is measured its size with digital display calliper behind the sintering, calculates shrinking percentage; Behind even coiling 20 circles of copper cash with line footpath 0.3mm, with TH2828LCR tester (1K～1MHz) inductance measuring and Q value; Utilize Archimedes's drainage bulk density, the performance perameter of the sample that obtains sees Table 3.
Figure BDA0000033251180000061
Table 3
As can be seen from Table 3, under (1) same calcined temperature, along with the raising of sintering temperature, sintered density increases, and average grain size increases, and grain size becomes evenly μ iAlso increase thereupon; (2) improve calcined temperature, the powder active variation, thus have influence on the growth of later stage crystal grain during sintering and the raising of density, in addition, calcined temperature is too high, also can cause the discontinuous growth of crystal grain in the later stage sintering process, causes μ iReduce.
Above example explanation, the present invention has obtained the laminated inductive material of low-cost and high-performance, by adding a small amount of sintering agent, and the low-temperature sintering under having realized 900 ℃, the material sintering character is good, porcelain body density height, epigranular is by prescription and technology adjustment, the initial permeability of material has covered 20～400 a series, quality factor q is higher, and test shows that material of the present invention is that performance has the laminated inductive material of wide application prospect preferably in the lower cost materials.
The above only is embodiments of the invention; be not so limit claim of the present invention; every equivalent structure or equivalent flow process conversion that utilizes specification sheets of the present invention and accompanying drawing content to be done; or directly or indirectly be used in other relevant technical fields, all in like manner be included in the scope of patent protection of the present invention.

Claims (8)

1. low-temperature sintering soft magnetic ferrite, it is characterized in that: the major ingredient of described low-temperature sintering soft magnetic ferrite is the magnesium copper zinc ferrite, the auxiliary material of described low-temperature sintering soft magnetic ferrite is bismuth oxide and cobalt oxide; Major ingredient shared mass percent in prescription is 95～99%, and auxiliary material shared mass percent in prescription is 1～5%.
2. low-temperature sintering soft magnetic ferrite according to claim 1 is characterized in that, described magnesium copper zinc ferrite, and the molar percentage of each component is as follows:
Fe 2O 3： 47％～50％；
Magnesium basic carbonate in MgO: 7%～37%;
ZnO： 4％～31％；
CuO： 6％～14％。
3. the preparation method of low-temperature sintering soft magnetic ferrite according to claim 1 and 2 is characterized in that, may further comprise the steps:
1) takes by weighing Fe 2O 3, ZnO, CuO and magnesium basic carbonate;
2), the gained slurry in 120～150 ℃ of oven dry down, is crossed 200 mesh sieves with step 1) products therefrom and deionized water mixed grinding form slurry;
3) with step 2) the back gained powder that sieves places sintering oven in 800～875 ℃ of following pre-burnings, is incubated 2～4 hours;
4) mixed that the pre-burning product of step 3) gained and bismuth oxide and cobalt oxide are provided by claim 1 or 2 grinds to form slurry with mix products and deionized water, and the gained slurry in 120～150 ℃ of oven dry down, is crossed 200 mesh sieves;
5) step 4) is sieved back gained powder adds tackiness agent PVA and granulation, compression moulding;
6) with the product of step 5) compression moulding at 860～950 ℃ of following sintering 4～6h.
4. according to the preparation method of the described low-temperature sintering soft magnetic ferrite of claim 3, it is characterized in that:
Step 2) or 4) described grinding is: raw material that will be to be ground mixes back ball milling 2～3h in planetary ball mill with deionized water and zirconium post.
5. according to the preparation method of the described low-temperature sintering soft magnetic ferrite of claim 3, it is characterized in that:
In the described compression moulding step of step 5), its forming pressure is 6MPa, pressurize 10～15s.
6. a magnesium copper zinc ferrite is characterized in that, described magnesium copper zinc ferrite, and the molar percentage of each component is as follows:
Fe 2O 3： 47％～50％；
Magnesium basic carbonate in MgO: 7%～37%;
ZnO： 4％～31％；
CuO： 6％～14％。
7. the preparation method of magnesium copper zinc ferrite according to claim 6 is characterized in that, may further comprise the steps:
1) gets Fe by stoichiometric ratio 2O 3, ZnO, CuO and magnesium basic carbonate;
2), the gained slurry in 120～150 ℃ of oven dry down, is crossed 200 mesh sieves with step 1) products therefrom and deionized water mixed grinding form slurry;
3) with step 2) the back gained powder that sieves places sintering oven in 800～875 ℃ of following pre-burnings, is incubated 2～4 hours.
8. the preparation method of magnesium copper zinc ferrite according to claim 7 is characterized in that: step 2) described grinding is: raw material that will be to be ground mixes back ball milling 2～3h in planetary ball mill with deionized water and zirconium post.
CN 201010551863 2010-11-19 2010-11-19 Low-temperature sintering soft magnetic ferrite material, magnesium, copper and zinc ferrite and preparation methods thereof Pending CN102050622A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102424583A (en) * 2011-09-05 2012-04-25 吕佳佳 Magnetic powder for bonding hard ferrite
CN102531560A (en) * 2011-12-30 2012-07-04 南通鼎源电子磁材有限公司 Magnetism, copper and zinc-iron soft magnetic ferrite material and preparation method thereof
CN103896571A (en) * 2014-03-01 2014-07-02 南通万宝实业有限公司 Permanent magnetic ferrite material with high magnetic energy
CN106977193A (en) * 2017-04-27 2017-07-25 湖北高磁新材料科技有限公司 A kind of Ferrite Material and its manufacture method for laminated sheet inductance

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102424583A (en) * 2011-09-05 2012-04-25 吕佳佳 Magnetic powder for bonding hard ferrite
CN102531560A (en) * 2011-12-30 2012-07-04 南通鼎源电子磁材有限公司 Magnetism, copper and zinc-iron soft magnetic ferrite material and preparation method thereof
CN103896571A (en) * 2014-03-01 2014-07-02 南通万宝实业有限公司 Permanent magnetic ferrite material with high magnetic energy
CN103896571B (en) * 2014-03-01 2015-10-14 南通万宝实业有限公司 A kind of high magnetic energy permanent-magnet ferrite material
CN106977193A (en) * 2017-04-27 2017-07-25 湖北高磁新材料科技有限公司 A kind of Ferrite Material and its manufacture method for laminated sheet inductance

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