CN1304894A - Process for preparing cordierite-base microcrystal glass-ceramics medium material used for multi-layer inductor - Google Patents

Process for preparing cordierite-base microcrystal glass-ceramics medium material used for multi-layer inductor Download PDF

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Publication number
CN1304894A
CN1304894A CN 01102209 CN01102209A CN1304894A CN 1304894 A CN1304894 A CN 1304894A CN 01102209 CN01102209 CN 01102209 CN 01102209 A CN01102209 A CN 01102209A CN 1304894 A CN1304894 A CN 1304894A
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glass
hour
cordierite
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layer inductor
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CN1120812C (en
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周和平
罗凌虹
查征
王少洪
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Tsinghua University
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Tsinghua University
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/097—Glass compositions containing silica with 40% to 90% silica, by weight containing phosphorus, niobium or tantalum

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

A cordierite-based microcrystal glass/ceramic dielectric material for multi-layer inductor is prepared through mixing MgO, Al2O3, SiO2, B2O3 and P2O5, adding alcohol, mixing, drying, melting to prepare glass, quenching, wet ball grinding, die pressing to obtain wafer, and calcining. Its advantages are low-temp (lower than 1000 deg.C) sinteing it with Au, Ag/Pd, or Cu electrode, low dielectric constant and low dielectric loss.

Description

A kind of preparation method of cordierite-base microcrystal glass-ceramics medium material used for multi-layer inductor
The present invention relates to a kind of preparation method of cordierite-base microcrystal glass-ceramics medium material used for multi-layer inductor, belong to materials science field.
The dielectric material of traditional lamellar inductor generally adopts the Ferrite Material of soft magnetism, and soft magnetic iron magnet (ferrite) has three kinds of crystal formations commonly used, is respectively spinel type, carbuncle type and Magnetoplumbate-type.In the ferrite of spinel type, the NiZn ferrite has obtained extensive studies and application the most.Some other system, such as, Li based ferrite, MgZn ferrite, MnZn ferrite also have been subjected to scholar's attention and research, but these systems are because the restriction of self frequency aspect can not be used for high frequency.Y iron garnet (YIG) is the representative of garnet type ferrite, and magnetic magneto-plumbite type ferrites is representative with the Ba ferrite then.These two kinds of Ferrite Materials are not used for producing in a large number, and the research of carrying out at them is still arranged in the scholar.The NiZnCu ferrite be in industry, use at present the most a kind of dielectric material, it is formed by part Ni and the Zn that Cu has substituted in the NiZn ferrite, the crystal formation of spinel does not change.More common molecular formula is as Ni 0.25Cu 0.25Zn 0.50Fe 2O 4, CuO adds wherein as a kind of low-temperature metal oxide compound, and purpose is to reduce ferritic sintering temperature.To the NiZnCu ferrite, sintering temperature drops to 1050 ℃ from 1250 ℃ from the NiZn ferrite.Then,, again temperature is reduced, thereby be implemented in sintering below 900 ℃ by other way.For the effect that Cu is played therein, also there are a lot of scholars to do corresponding research.Wherein noticeable with the research of Japanese scholar Fujimoto.In fact, in order to reduce the sintering temperature of NiZnCu, various ways have been tested by scholar and manufacturer.Main experiment can reduce two classes; (1) reduces sintering temperature by adding some fusing assistants.As, add Bi 2O 3Or Pb glass.(2) way by the preparation ultrafine powder reduces sintering temperature.As, efflorescence again after the pre-burning perhaps adopts the chemical process of sol-gel to prepare raw material [13-14].Recently, the method that the scholar who has has tested the xerogel auto-combustion prepares ferritic ultrafine powder, has obtained reasonable result.The NiZnCu ferrite is that as the advantage of dielectric material its magnetic permeability is bigger, can arrive hundreds of to several thousand, but it can not be used for high frequency and ultra-high frequency (500MHz-5GMHz), its reason is: the electric medium constant of this dielectric material is big (being generally 10-15), makes lamellar inductor produce bigger subsidiary electric capacity under high frequency; Its inductance value is also bigger simultaneously, and the self-resonant frequency of inducer determines that by inductance value and subsidiary electric capacity its relational expression is: SRF=1/[2 π (LC p) 1/2].Inductance (L) and electric capacity (Cp) are big more, and self-resonant frequency is more little on the contrary.So the multilayer chip inductor that is dielectric material with this traditional Ferrite Material can't be applicable to utmost point radio band.
The development trend of electronic product can reduce " Four Modernizations " roughly now, i.e. miniaturization, mobile, digitizing and high frequencyization.And for many years, the technical development of inducer relatively lags behind, and has influenced the overall development of electronic product.Chip inductor mainly is divided into two classes: multi-layer type chip inductor and wire-wound chip inductor device.In market that the expert did was estimated, both portions were respectively 60% and 40%, and along with the development of technology, the former will increase by shared proportion gradually.The major advantage of lamellar inductor (MLCI) has: volume is little; The reliability height; Magnetic shielding is good; Be suitable for surface mounting (SMT) and automatic assembling etc.Many electronic products all be unable to do without lamellar inductor, as notebook, cell-phone, beeper, large-screen color TV movement etc.The application of lamellar inductor comprises: (1) and the synthetic LC wave filter of electric capacity; (2) conduct exchanges obstructing instrument in active device (as transistor); (3) be used for matching circuit; (4) as anti-electromagnetic interference (EMI) wave filter.Aspect the research and industrialization of multilayer tablet sense, Japan is walked in front, the world.As far back as 1986, they just proposed original sheet sense design, and in subsequently several years, constantly study and improve the technology of sheet sense.At present, the manufacturer of Japan has occupied most of market, and especially aspect frequency applications, TDK company, field, village company, company of TAIYO YUDAN and the TOKO company of Japan all have self-resonant frequency to be higher than the 4GHz product.The level of the U.S. is only second to Japan.Be Korea S and Taiwan backward.Domestic will falling behind relatively, but in recent years, existing part scholar has carried out fruitful research.
In sheet sensor spare, mainly contain two kinds of materials: electrode materials and dielectric material.Wherein electrode materials generally adopts argent (Ag) or silver-palladium alloy (Ag-Pd), and argent is to be chosen as the conductor of Inside coil owing to having minimum resistivity, if adopt argent, dielectric material requires sintering below 900 ℃; If dielectric material is at 1000 ℃ of following sintering, then adopt silver-colored palladium electrode, so, the low fever's dielectric material that is used for chip inductor is the gordian technique of chip inductor, frequently from present research and industrialized present situation, low fever's dielectric material that present chip inductor is used mainly contains three classes, and a class is to be applied to the ferrite medium of 300MHz with lower frequency; Another kind of is stupalith and the ferritic miscellany that is applied to the low-k in the high-frequency range (500MHz-2GHz); The 3rd class is low-k (1MHz, K＜5.0 that are applied in the uhf region (2-5GHz); 1MHZ, tan δ＜0.001) stupalith dielectric material.
In the research of low Jie's porcelain, Taiwan's scholars is permitted positive source (Jen-Yan Hsu) and has been delivered one piece of very important article in 1997, mentions them and has prepared three groups of samples with low Jie's porcelain and experimentize, and has obtained 5.3 to the 2.4GHz high frequency.But in this literary composition, he does not spell out the system of the low Jie's porcelain that is adopted, and has just listed several conditions, as low medium electric constant (ε r=4-5), low loss tangent (at 1MHz, tan δ≤0.001) and low sintering temperature (being lower than 900 ℃).
Along with the continuous development of microelectronics, as mobile phone, hand-held computer, products such as large color screen movement are constantly to the high frequency development now, and it is extremely urgent to produce the electronic devices and components that are suitable for high frequency, ultra-high frequency application.This has higher requirement to corresponding electronic device material, and for many years, the technical development of inducer relatively lags behind, and has influenced the overall development of electronic product.
The objective of the invention is to propose a kind of preparation method of cordierite-base microcrystal glass-ceramics medium material used for multi-layer inductor, select the dielectric material of a kind of nonmagnetic ceramic materials as the high-frequency chip inductor device, and adopted devitrified glass technology to reach low sintering purpose so that be lower than 1000 ℃ down and Ag, Au, electrodes such as Ag/Pd, Cu burn altogether.Adopt this new material to make inducer as the dielectric material and the novel process of chip inductor, this chip inductor is expected to use under the ultra-high frequency of 2-5GHz.
The preparation method of the cordierite-base microcrystal glass-ceramics medium material used for multi-layer inductor that the present invention proposes may further comprise the steps:
1, with the following column weight amount of raw material percentage mix: MgO (5-25wt%), Al 2O 3(20-25wt%), SiO 2(50-70wt%), B 2O 3(1-5wt%) and P 2O 5(1-5wt%) (B wherein 2O 3With H 2BO 3Form is introduced, P 2O 5With NH 4H 2PO 4Form is introduced);
2, add ethanol in above-mentioned compound, additional proportion is: compound and alcoholic acid weight ratio are 1.5-2.5, after wet-mixed 3-5 hour, descended dry 2-3 hour at 60-80 ℃, in the high alumina crucible of packing into, fusion cast glass, glass melting temperature is 1400-1600 ℃, is incubated 2-4 hour;
3, will obtain transparent vitreum behind the glass quenching, wet ball grinding glass to median size is 0.5-2.0 μ m, at the molded one-tenth sequin of the pressure of 100-120MPa, burns till under 850-1050 ℃, and soaking time is 2-6 hour, promptly obtains material of the present invention.
The advantage of the inventive method is:
Adopted B 2O 3-P 2O 5-MgO-Al 2O 3-SiO 2System, and dielectric material, especially this material that cordierite glass-ceramic technology is made the high-frequency multilayer chip inductor can be lower than under 1000 ℃ of temperature and Au, Ag/Pd, the Cu electrode burns and sinters into requirement (DIELECTRIC CONSTANT=5.7, the 1MHz that porcelain reaches low-k and low-dielectric loss altogether; Dielectric loss tan δ=0.0013,1MHz).
(1) this patent has selected trichroite (its specific inductivity is 4.5) to be the principal crystalline phase of dielectric material in numerous low Jie's porcelain, and boron (phosphorus) silicate glass is glassy phase (specific inductivity of borate glass is 3.7).
(2) owing to introduced B 2O 3And P 2O 5Chemical reagent has not only promoted crystallization but also accelerated densification process, has reduced the agglomerating temperature.Boron trioxide can reduce the high temperature viscosity of glass, promotes the densification process of glass; Because the asymmetry of Vanadium Pentoxide in FLAKES molecular structure but it usually becomes a kind of crystallization agent of glass.Add an amount of B in this experiment 2O 3And P 2O 5, reached the purpose of low-temperature sintering cordierite glass-ceramic, and most of crystal exists with the α-Jin Qingshi form and a spot of boron (phosphorus) silicate glass.This is very favourable to the specific inductivity and the dielectric loss that reduce material.
Embodiments of the invention.
Embodiment 1:
Weighing MgO (8.5wt%), Al 2O 3(21.5wt%), SiO 2(70wt%), B 2O 3(2.5wt%) and P 2O 5(2.5wt%) (B wherein 2O 3With H 2BO 3Form is introduced, P 2O 5With NH 4H 2PO 4Form is introduced), add (60 ℃ of adequate amount of ethanol (material is 1.5 with the alcoholic acid weight ratio) wet-mixed 3hr after drying, 2hr), pack in the high alumina crucible fusion cast glass (1450 ℃ of insulations, 4 hours) into, transparent vitreum will be obtained behind the glass quenching, wet ball grinding glass to median size is 0.8 μ m, at the dry-pressing formed one-tenth sequin of the pressure of 100MPa, burns till by the firing temperature of formulating that (maximum sintering temperature is 880 ℃; Soaking time is 4 hours), promptly obtain material of the present invention.
Embodiment 2:
Weighing MgO (15wt%), Al 2O 3(25wt%), SiO 2(60wt%), B 2O 3(0.5wt%) and P 2O 5(0.5wt%) (B wherein 2O 3With H 2BO 3Form is introduced, P 2O 5With NH 4H 2PO 4Form is introduced), add (70 ℃ of adequate amount of ethanol (material is 2.0 with the alcoholic acid weight ratio) wet-mixed 4hr after drying, 3hr), pack in the high alumina crucible fusion cast glass (1500 ℃ of insulations, 2 hours) into, transparent vitreum will be obtained behind the glass quenching, wet ball grinding glass to median size is 0.67 μ m, at the dry-pressing formed one-tenth sequin of the pressure of 110MPa, burns till by the firing temperature of formulating that (maximum sintering temperature is 900 ℃; Soaking time is 3 hours), promptly obtain material of the present invention.
Embodiment 3:
Weighing MgO (20wt%), Al 2O 3(25wt%), SiO 2(55wt%), B 2O 3(1.5wt%) and P 2O 5(1.5wt%) (B wherein 2O 3With H 2BO 3Form is introduced, P 2O 5With NH 4H 2PO 4Form is introduced), add (80 ℃ of adequate amount of ethanol (material is 2.0 with the alcoholic acid weight ratio) wet-mixed 4hr after drying, 3hr), pack in the high alumina crucible fusion cast glass (1550 ℃ of insulations, 2 hours) into, transparent vitreum will be obtained behind the glass quenching, wet ball grinding glass to median size is 1.42 μ m, at the dry-pressing formed one-tenth sequin of the pressure of 115MPa, burns till by the firing temperature of formulating that (maximum sintering temperature is 950 ℃; Soaking time is 4 hours), promptly obtain material of the present invention.
Embodiment 4:
Weighing MgO (25wt%), Al 2O 3(25wt%), SiO 2(50wt%), B 2O 3(4.5wt%) and P 2O 5(4.5wt%) (B wherein 2O 3With H 2BO 3Form is introduced, P 2O 5With NH 4H 2PO 4Form is introduced), add (75 ℃ of adequate amount of ethanol (material is 1.8 with the alcoholic acid weight ratio) wet-mixed 3.5hr after drying, 2hr), pack in the high alumina crucible fusion cast glass (1600 ℃ of insulations, 1 hour) into, transparent vitreum will be obtained behind the glass quenching, wet ball grinding glass to median size is 1.02 μ m, at the dry-pressing formed one-tenth sequin of the pressure of 120MPa, burns till by the firing temperature of formulating that (maximum sintering temperature is 1020 ℃; Soaking time is 2 hours), promptly obtain material of the present invention.

Claims (1)

1, a kind of preparation method of cordierite-base microcrystal glass-ceramics medium material used for multi-layer inductor, this method may further comprise the steps:
(1) with the following column weight amount of raw material percentage mix:
MgO 5-25wt％
Al 2O 3 20-25wt％
SiO 2 50-70wt％
B 2O 3 1-5wt％
P 2O 5 1-5wt％
(2) add ethanol in above-mentioned compound, additional proportion is: compound and alcoholic acid weight ratio are 1.5-2.5, after wet-mixed 3-5 hour, descended dry 2-3 hour at 60-80 ℃, in the high alumina crucible of packing into, fusion cast glass, glass melting temperature is 1400-1600 ℃, is incubated 2-4 hour;
(3) will obtain transparent vitreum behind the glass quenching, wet ball grinding glass to median size is 0.5-2.0 μ m, at the molded one-tenth sequin of the pressure of 100-120MPa, burns till under 850-1050 ℃, and soaking time is 2-6 hour, promptly obtains material of the present invention.
CN 01102209 2001-01-18 2001-01-18 Process for preparing cordierite-base microcrystal glass-ceramics medium material used for multi-layer inductor Expired - Fee Related CN1120812C (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7034637B2 (en) 2003-04-21 2006-04-25 Murata Manufacturing Co., Ltd. Electronic component
CN101148323B (en) * 2007-09-06 2010-06-16 北京科技大学 Low-temperature co-fired cordierite series glass-ceramic substance power and preparation method thereof
CN101503307B (en) * 2009-02-27 2010-11-10 航天材料及工艺研究所 Dielectric property acceleration stabilization method for silicon dioxide based composite material
CN103641463A (en) * 2013-12-05 2014-03-19 湖南省新化县长江电子有限责任公司 Ceramic tube for explosionproof fuse for automobile and preparation method of ceramic tube
CN105271763A (en) * 2015-11-20 2016-01-27 中国地质大学（武汉） Low-dielectric low-expanded cordierite glass-ceramic material taking perlite as main raw materials and preparation method thereof
WO2019191350A1 (en) * 2018-03-28 2019-10-03 Corning Incorporated Boron phosphate glass-ceramics with low dielectric loss
CN111170634A (en) * 2020-01-10 2020-05-19 浙江大学 High-alumina phosphosilicate glass suitable for chemical strengthening and chemically toughened glass
CN111320391A (en) * 2020-03-04 2020-06-23 景德镇陶瓷大学 Colorless transparent cordierite glass ceramic and preparation method thereof

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7034637B2 (en) 2003-04-21 2006-04-25 Murata Manufacturing Co., Ltd. Electronic component
CN101148323B (en) * 2007-09-06 2010-06-16 北京科技大学 Low-temperature co-fired cordierite series glass-ceramic substance power and preparation method thereof
CN101503307B (en) * 2009-02-27 2010-11-10 航天材料及工艺研究所 Dielectric property acceleration stabilization method for silicon dioxide based composite material
CN103641463A (en) * 2013-12-05 2014-03-19 湖南省新化县长江电子有限责任公司 Ceramic tube for explosionproof fuse for automobile and preparation method of ceramic tube
CN105271763A (en) * 2015-11-20 2016-01-27 中国地质大学（武汉） Low-dielectric low-expanded cordierite glass-ceramic material taking perlite as main raw materials and preparation method thereof
CN105271763B (en) * 2015-11-20 2017-11-24 中国地质大学（武汉） It is a kind of using perlite as low Jie's low bulk cordierite glass-ceramic material of primary raw material and preparation method thereof
WO2019191350A1 (en) * 2018-03-28 2019-10-03 Corning Incorporated Boron phosphate glass-ceramics with low dielectric loss
CN111971257A (en) * 2018-03-28 2020-11-20 康宁股份有限公司 Borophosphate glass ceramics with low dielectric loss
US11236012B2 (en) 2018-03-28 2022-02-01 Corning Incorporated Boron phosphate glass-ceramics with low dielectric loss
CN111170634A (en) * 2020-01-10 2020-05-19 浙江大学 High-alumina phosphosilicate glass suitable for chemical strengthening and chemically toughened glass
CN111320391A (en) * 2020-03-04 2020-06-23 景德镇陶瓷大学 Colorless transparent cordierite glass ceramic and preparation method thereof
CN111320391B (en) * 2020-03-04 2021-09-24 景德镇陶瓷大学 Colorless transparent cordierite glass ceramic and preparation method thereof

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