CN108314327A - Ce adulterates low-temperature co-burning ceramic material and preparation method thereof - Google Patents

Ce adulterates low-temperature co-burning ceramic material and preparation method thereof Download PDF

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CN108314327A
CN108314327A CN201810045899.7A CN201810045899A CN108314327A CN 108314327 A CN108314327 A CN 108314327A CN 201810045899 A CN201810045899 A CN 201810045899A CN 108314327 A CN108314327 A CN 108314327A
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ceramic material
low
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burning ceramic
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CN108314327B (en
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韩娇
曾明
曾一明
向遥
李世鸿
李文琳
刘继松
白培加
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Sino Platinum Metals Co Ltd
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    • C03C12/00—Powdered glass; Bead compositions
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    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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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
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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
    • C04B35/63—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 using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632—Organic additives
    • C04B35/634—Polymers
    • C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B35/63416—Polyvinylalcohols [PVA]; Polyvinylacetates
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    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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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
    • C04B35/63—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 using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/638—Removal thereof
    • C—CHEMISTRY; METALLURGY
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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
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
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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
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
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    • 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
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3409—Boron oxide, borates, boric acids, or oxide forming salts thereof, e.g. borax
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    • C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient

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Abstract

The invention discloses Ce to adulterate low-temperature co-burning ceramic material and preparation method thereof, belongs to electronic information function Material Field, and in particular to a kind of low-temperature co-burning ceramic material and preparation method thereof.Ceramic material of the present invention is by the glass powder (CaO, 10~20% B that mass percentage is 30~50%2O3, 35~45% SiO2, 0~20% CeO2It is prepared through ball mill grinding sieving drying through high-temperature fusion water quenching) compression moulding is sintered.Glass powder powder density ranging from 2.8~3.3g/cm used in ceramic material of the present invention3, softening range is 710~750 DEG C, and Ceramics Material Heat Expansion Coefficient is 6.5~8.0 × 10‑6Within the scope of ppm/ DEG C, dielectric constant is adjustable in 4~8.5 ranges, and dielectric loss is 0.9~1.2 × 10‑3Minor fluctuations in range.

Description

Ce adulterates low-temperature co-burning ceramic material and preparation method thereof
Technical field
The invention belongs to electronic information function Material Fields, are related to a kind of ltcc substrate material, and in particular to a kind of low temperature Material of ceramics burned together and preparation method thereof.
Background technology
Low-temperature co-fired ceramics (low temperature co-fired ceramics, LTCC) technology is sealed with its modularization The characteristics of filling and can be with metal electrode low-temperature matching co-firing was widely used in large scale integrated circuit envelope for over ten years in the past Dress, radar, antenna and high-frequency wireless communication field, it is the High Density Integration of passive electronic components and system-level complete electronic set envelope Dress provides ideal technology platform.Currently, the development of the passive element based on ceramic material is relatively slow, passive element Modularization and it is integrated cannot meet always semiconductor technology fast development the needs of, have become semiconductor technology development " bottleneck ".And as applied to one of most important baseplate material in high-frequency communication field, calcium borosilicate (CaO-B2O3-SiO2, CBS) Microcrystalline glass in series has a series of excellent performances, such as：Relatively low sintering temperature (<900 DEG C), extremely low dielectric constant (εr<And dielectric loss (tan δ 6.5)<1×10-3), therefore as one of most important ltcc substrate material.
With the fast development of high-frequency wireless communication and microelectronic packaging technology, LTCC technology and microwave dielectric material are carried Higher requirement is gone out, including higher packaging density, broader process window, higher mechanical strength, lower dielectric are normal Number and dielectric loss etc..But object phase transformation during CBS systems baseplate material there are process windows narrow, mechanical strength is not high and cofiring Change the shortcomings of complicated, with the fast development of high-frequency communication technology, existing CBS baseplate materials comprehensive performance is increasingly difficult to meet The market demand.Therefore, exploitation possesses independent intellectual property right, suitable for low temperature co-fired new material, and it is low temperature co-fired to become China instantly China industry development one of must solve the problems, such as.
Invention content
The purpose of the present invention is to provide the controllable a kind of low temperature of a kind of sintering temperature, dielectric properties and coefficient of thermal expansion is total Burning ceramic material and preparation method thereof.
Ce doping low-temperature co-burning ceramic material of the present invention follows these steps to realize：
One, the preparation of the CBS glass powders of doping Ce
1) equal batch mixing is prepared：The CaO, 10~20% B that good quality percentage composition is 30~50% are weighed in proportion2O3, 35 ~45% SiO2, 0~20% CeO2, and each raw material is sufficiently mixed uniformly, it is configured to equal batch mixing；
2) above-mentioned equal batch mixing is placed in platinum crucible, heats and melts in 1300~1500 DEG C of resistance furnace, heat preservation 2~ 4h obtains the glass metal of uniform component；
3) by the glass metal melted in pouring into deionized water, its quick quenching is made to form glass through high-temperature fusion water quenching Glass particle；
4) by obtained vitreum in planetary ball mill 8~12h of ball milling, the material after ball milling is then crossed into 500 mesh Sieve, the drying to obtain present invention adulterate the CBS glass powders of Ce.
The glass frit component is uniform, and preparation temperature is 1300~1500 DEG C, and Ball-milling Time is 8~12h, crosses 500 mesh sieve, Drying temperature is 80 DEG C.
The glass powder powder density ranging from 2.8~3.3g/cm3。
3 μm~8 μm of the glass powder particle size range.
The glass powder softening point range is 710~750 DEG C.
It is prepared by the low-temperature co-burning ceramic material for two, mixing Ce
Binder PVA is added in the glass powder that step 1 obtains to be granulated, then compression moulding under a certain pressure is put Normal pressure is sintered 10~30min with 750 DEG C~850 DEG C of temperature after dumping on sintering gasket, is mixed after natural cooling The low-temperature co-burning ceramic material of Ce.
The Ceramics Material Heat Expansion Coefficient is 7.6~8.0 × 10-6Within the scope of ppm/ DEG C.
The ceramic dielectric constant is adjustable in 4~8.5 ranges, and dielectric loss is 0.9~1.2 × 10-3In range Minor fluctuations.
Description of the drawings
Fig. 1 is the DSC curve of 1 glass powder of present example.
Fig. 2 is the thermal dilatometry of 1 ceramic material of present example.
Specific implementation mode
In order to preferably explain the present invention, with reference to the embodiment specific implementation mode that the present invention is furture elucidated and carefully Section, but present disclosure is not limited solely to embodiment described below, it is all done according to spirit of the invention it is equivalent Changes or modifications should be covered by the protection scope of the present invention.
Embodiment 1
(1) it is by mass percent：CaO 38%, B2O315%, SiO242%, CeO25% raw material is sufficiently mixed Uniformly, it is configured to equal batch mixing；
(2) prepared equal batch mixing is packed into platinum crucible, keeps the temperature 2~4h at 1400 DEG C in resistance furnace, then will melts Molten glass metal makes its quick quenching form vitreum in pouring into deionized water；
(3) by obtained vitreum in planetary ball mill with 450rpm ball milling 12h, then by the material mistake after ball milling 500 mesh sieve, 80 DEG C of drying to obtain glass powders；
(4) glass powder is subjected to dsc analysis test (as shown in Figure 1), glass powder density is 2.97g/cm3, softening point is 721℃；
(5) appropriate glass powder is taken, PVA is added and is granulated, and in the pressure lower sheeting of 70~100Mpa, the green compact pressed are existed 2h dumpings are kept the temperature at 600 DEG C, then carry out 15~20min of solid-phase sintering under air atmosphere at 750-850 DEG C to get to ceramics Dielectric material.
(6) coefficient of thermal expansion is carried out to gained dielectric material and dielectric properties is tested, Coefficient of Thermal Expansion value is：8.0×10- 6Ppm/ DEG C, dielectric constant 5.8, dielectric loss is 1.2 × 10-3。
Embodiment 2
(1) it is by mass percent：CaO 33%, B2O312%, SiO235%, CeO220% raw material is sufficiently mixed Uniformly, it is configured to equal batch mixing；
(2) prepared equal batch mixing is packed into platinum crucible, keeps the temperature 2~4h at 1400 DEG C in resistance furnace, then will melts Molten glass metal makes its quick quenching form vitreum in pouring into deionized water；
(3) by obtained vitreum in planetary ball mill with 450rpm ball milling 12h, then by the material mistake after ball milling 500 mesh sieve, 80 DEG C of drying to obtain glass powders；
(4) glass powder is subjected to dsc analysis test, glass powder density is 3.26g/cm3, softening point is 717 DEG C；
(5) appropriate glass powder is taken, PVA is added and is granulated, and in the pressure lower sheeting of 70~100Mpa, the green compact pressed are existed 2h dumpings are kept the temperature at 600 DEG C, then carry out 15~20min of solid-phase sintering under air atmosphere at 750-850 DEG C to get to ceramics Dielectric material.
(6) coefficient of thermal expansion is carried out to gained dielectric material and dielectric properties is tested, Coefficient of Thermal Expansion value is：7.8×10- 6Ppm/ DEG C, dielectric constant 4.1, dielectric loss is 1.1 × 10-3。

Claims (6)

1.Ce adulterates the preparation method of low-temperature co-burning ceramic material, it is characterised in that follows these steps to realize：
One, the CaO, 10~20% B for being 30~50% by mass percentage2O3, 35~45% SiO2, 0~20% CeO2It is uniformly mixed to obtain equal batch mixing, water quenching, ball milling drying, which prepare to process, after high-temperature fusion obtains the CBS glass powders of doping Ce；
Two, then the glass powder compression moulding for obtaining step 1 is placed on sintering gasket under normal pressure with 750 DEG C~850 DEG C Temperature is sintered 10~30min, obtains mixing the low-temperature co-burning ceramic material of Ce after natural cooling.
2. the preparation method of Ce doping low-temperature co-burning ceramic material as described in claim 1, it is characterised in that：The step 1 High temperature melts：Prepared equal batch mixing is packed into platinum crucible, keeps the temperature 2~4h at 1300~1500 DEG C in resistance furnace.
3. the preparation method of Ce doping low-temperature co-burning ceramic material as described in claim 1, it is characterised in that：The step 1 Middle ball milling is dried：By obtained vitreum with 450rpm ball milling 12h in planetary ball mill, then by the material after ball milling Cross 500 mesh sieve, 80 DEG C of drying to obtain glass powders.
4. the preparation method of Ce doping low-temperature co-burning ceramic material as described in claim 1, it is characterised in that：The step 2 Middle compression moulding is：Appropriate glass powder is taken, PVA is added and is granulated, and in the pressure lower sheeting of 70~100Mpa, the green compact that will be pressed 2h dumpings are kept the temperature at 600 DEG C.
5.Ce adulterates the preparation method of low-temperature co-burning ceramic material, it is characterised in that follows these steps to realize：
(1) it is by mass percent：CaO 33%, B2O312%, SiO235%, CeO220% raw material is sufficiently mixed uniformly, It is configured to equal batch mixing；
(2) prepared equal batch mixing is packed into platinum crucible, keeps the temperature 2~4h at 1400 DEG C in resistance furnace, it then will be molten Glass metal makes its quick quenching form vitreum in pouring into deionized water；
(3) by obtained vitreum in planetary ball mill with 450rpm ball milling 12h, the material after ball milling is then crossed 500 Mesh sieves, 80 DEG C of drying to obtain glass powders；
(4) glass powder is subjected to dsc analysis test, glass powder density is 3.26g/cm3, softening point is 717 DEG C；
(5) appropriate glass powder is taken, PVA is added and is granulated, and in the pressure lower sheeting of 70~100Mpa, by the green compact pressed 600 2h dumpings are kept the temperature at DEG C, 15~20min of solid-phase sintering is then carried out under air atmosphere at 750-850 DEG C is situated between to get to ceramics Material；
(6) coefficient of thermal expansion is carried out to gained dielectric material and dielectric properties is tested, Coefficient of Thermal Expansion value is：7.8×10-6ppm/ DEG C, dielectric constant 4.1, dielectric loss is 1.1 × 10-3。
6. Ce described in any one of claim 1 to 5 adulterates low-temperature co-burning ceramic material, it is characterised in that：The Ce adulterates low temperature Material of ceramics burned together mass percentage is：30~50% CaO, 10~20% B2O3, 35~45% SiO2, 0~20% CeO2, CBS glass powders powder density ranging from 2.8~3.3g/cm of the Ce doping3, glass powder softening point range is 710~750 DEG C, recrystallization temperature is 780~850 DEG C；Coefficient of thermal expansion is 6.5~8.0 × 10-6Within the scope of ppm/ DEG C；Dielectric is normal Number is adjustable in 4~8.5 ranges, and dielectric loss is 0.9~1.2 × 10-3Range.
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Cited By (3)

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Publication number Priority date Publication date Assignee Title
CN112624754A (en) * 2020-12-08 2021-04-09 赣州中瓷科技有限公司 LTCC ceramic powder for high-frequency capacitor and preparation process thereof
CN114656155A (en) * 2022-04-29 2022-06-24 中国科学院上海硅酸盐研究所 Low-dielectric low-loss low-expansion glass material and preparation method and application thereof
CN115466109A (en) * 2022-10-18 2022-12-13 昆明贵研新材料科技有限公司 Calcium-boron-silicon LTCC ceramic material and preparation method thereof

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EP2913311A1 (en) * 2014-02-26 2015-09-02 Heraeus Precious Metals North America Conshohocken LLC A glass comprising tungsten and lead in a solar cell paste
CN105924172A (en) * 2016-04-22 2016-09-07 天津大学 Rare earth doped ceramic-based diamond substrate material and preparation method thereof
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CN101148322A (en) * 2007-06-29 2008-03-26 清华大学 Microcrystal glass sealing material used for solid oxide fuel battery and sealing method thereof
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112624754A (en) * 2020-12-08 2021-04-09 赣州中瓷科技有限公司 LTCC ceramic powder for high-frequency capacitor and preparation process thereof
CN112624754B (en) * 2020-12-08 2022-11-29 赣州中傲新瓷科技有限公司 LTCC ceramic powder for high-frequency capacitor and preparation process thereof
CN114656155A (en) * 2022-04-29 2022-06-24 中国科学院上海硅酸盐研究所 Low-dielectric low-loss low-expansion glass material and preparation method and application thereof
CN114656155B (en) * 2022-04-29 2023-09-08 中国科学院上海硅酸盐研究所 Low-dielectric low-loss low-expansion glass material and preparation method and application thereof
CN115466109A (en) * 2022-10-18 2022-12-13 昆明贵研新材料科技有限公司 Calcium-boron-silicon LTCC ceramic material and preparation method thereof

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