CN108840666A - Low-temperature sintered microwave dielectric ceramic material and preparation method thereof - Google Patents

Low-temperature sintered microwave dielectric ceramic material and preparation method thereof Download PDF

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CN108840666A
CN108840666A CN201810812107.4A CN201810812107A CN108840666A CN 108840666 A CN108840666 A CN 108840666A CN 201810812107 A CN201810812107 A CN 201810812107A CN 108840666 A CN108840666 A CN 108840666A
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low
ceramic material
dielectric ceramic
microwave dielectric
temperature sintered
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CN108840666B (en
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孙兆海
张静
孙琳斐
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ZIBO YUHAI ELECTRONIC CERAMIC CO Ltd
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ZIBO YUHAI ELECTRONIC CERAMIC CO Ltd
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    • C—CHEMISTRY; METALLURGY
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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
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • 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
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/3258—Tungsten oxides, tungstates, or oxide-forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/3298—Bismuth oxides, bismuthates or oxide forming salts thereof, e.g. zinc bismuthate

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Abstract

The invention belongs to function ceramics fields, and in particular to a kind of low-temperature sintered microwave dielectric ceramic material and preparation method thereof.Chemical composition is BiW0.5Te3O12, low-temperature sintered microwave dielectric ceramic material of the present invention is with ultra-low sintering temperature (480~530 DEG C), low-k (26~30), high quality factor (6,754~13,120GHz), negative frequency-temperature coefficient (- 86~-197 × 10‑6/ DEG C), it can be used for MLCC offset-type baseplate material, have good commercial value, can be used for MLCC offset-type baseplate material；The present invention also provides preparation method, simple process, process is pollution-free, is suitable for industrialized production, has a extensive future.

Description

Low-temperature sintered microwave dielectric ceramic material and preparation method thereof
Technical field
The invention belongs to function ceramics fields, and in particular to a kind of low-temperature sintered microwave dielectric ceramic material and its preparation side Method.
Background technique
As the working frequency of communication equipment is further expanded to high-frequency range, after millimere-wave band, material Dielectric loss significantly increases, and signal transmission delay time is longer (signal delay time is directly proportional to dielectric constant), signal decaying Outstanding problem (dielectric loss is big, and Qf is low, and signal decaying is big).Developing, there are the microwave-medium ceramics of low dielectric constant and high Q f value to have It is significant.In addition, as microwave device is to high frequency, miniaturization, multi-functional, highly reliable, inexpensive development, LTCC skill Art is increasingly becoming the prefered method of high frequency substrate and integrated device application.
According to the properity feature and requirement of LTCC, LTCC with microwave-medium ceramics be broadly divided into ltcc substrate/ Encapsulating material and LTCC microwave device material two major classes.Ltcc substrate material should have sintering temperature and low, low-k, Low-dielectric loss and high insulation resistance etc..The research difficulty of baseplate material is big, core of the external each major company to investigation of materials Heart technical know-how, the research of domestic baseplate material are still at the initial stage, and the research of associated materials and technology of preparing is compared with foreign countries still There is gap.The ltcc substrate material being applied at present is mainly glass ceramics and devitrified glass, such as the BaO- of Murata company SiO2-Al2O3, ε 6.1, Qf 1500GHz；951 (Al of Dupont company2O3+CaZrO3+ glass), ε 7.8, Qf are 900GHz；MLS-25 (the Al of NEC Corporation2O3-B2O3-SiO2), ε 4.7, Qf 720GHz.One big limitation of these materials It is that Qf value is small, dielectric loss is big.
Summary of the invention
In view of the deficiencies of the prior art, the object of the present invention is to provide a kind of low-temperature sintered microwave dielectric ceramic material, tools There is a ultra-low sintering temperature, high Qf value, low-k, negative frequency-temperature coefficient can be used for MLCC offset-type baseplate material；This Invention also provides preparation method, and simple process, process is pollution-free, is suitable for industrialized production, has a extensive future.
Low-temperature sintered microwave dielectric ceramic material of the present invention, chemical composition BiW0.5Te3O12。
The preparation method of low-temperature sintered microwave dielectric ceramic material of the present invention, includes the following steps：
(1) by raw material Bi2O3、WO3、TeO2BiW is pressed respectively0.5Te3O12Chemical formula weighs ingredient；
(2) all raw materials are mixed, is put into ball grinder, ball milling, by the raw material stoving after ball milling, sieving；
(3) powder for obtaining step (2) is calcined at 400 ± 10 DEG C；
(4) PVA aqueous solution is added in step (3) calcined powder to be granulated, is sieved after drying, then with powder pressure Piece machine is pressed into cylinder；
(5) cylinder for obtaining step (4) is sintered in 480~530 DEG C, and Temperature Firing Microwave Dielectric Ceramics are made in heat preservation Material.
Wherein：
Raw materials used purity is all larger than 99.9%.
In step (2) Ball-milling Time be 4~6 hours, be sieved for 80 meshes.
Calcination time is 3 ± 0.1 hours in step (3).
PVA aqueous solution is the PVA aqueous solution that mass fraction is 5% in step (4).
The cylindrical cylinder for being Φ 12mm × 6mm in step (4).
The pressure of powder compressing machine is 8~12MPa in step (4).
Soaking time is 2~4 hours in step (5).
The low-temperature sintered microwave dielectric ceramic material being prepared is tested using tester, tester is network point Analyzer.
As a kind of most preferred technical solution, the preparation side of low-temperature sintered microwave dielectric ceramic material of the present invention Method includes the following steps：
(1) by Bi2O3、WO3、TeO2Respectively in molar ratio 1:0.5:3 weigh ingredient, and nylon tank is added raw materials into after mixing In, ball milling 6 hours；Raw material after ball milling is placed in infrared drying oven and dries, be sieved；
(2) it by the raw material after sieving, is calcined 3 hours in 400 DEG C；
(3) adding mass percent in powder after firing is that 5% PVA aqueous solution is granulated, and is sieved after drying, then The cylinder of Φ 12mm × 6mm is pressed into powder compressing machine；
(4) cylinder of step (3) is sintered in 520 DEG C, keeps the temperature 4 hours, ultralow-temperature sintering microwave medium ceramics are made；
(5) microwave dielectric property of microwave-medium ceramics made from testing procedure (4).
Its microwave dielectric property is：ε=29.1pC/N, Qf=13,120GHz, τf=-197 × 10-6/℃。
Compared with prior art, the present invention has the following advantages that：
(1) low-temperature sintered microwave dielectric ceramic material of the present invention is that one kind has high Qf value, low-k Microwave-medium ceramics.
(2) low-temperature sintered microwave dielectric ceramic material of the present invention has ultra-low sintering temperature (480~530 DEG C), Low-k (26~30), high quality factor (6,754~13,120GHz), negative frequency-temperature coefficient (- 86~-197 × 10-6/ DEG C) it can be used for MLCC offset-type baseplate material, have good commercial value.
(3) low-temperature sintered microwave dielectric ceramic material of the present invention has excellent microwave dielectric property, Neng Gouman Application of the sufficient microwave-medium ceramics in LTCC technology.
(4) the present invention also provides preparation methods, and simple process, process is pollution-free, are suitable for industrialized production, before Scape is wide.
Specific embodiment
Below with reference to embodiment, the present invention will be further described.
Embodiment 1-8
It is greater than 99.9% chemical raw material Bi using purity2O3、WO3、TeO2Prepare BiW0.5Te3O12Microwave-medium ceramics, Specific embodiment is as follows：
(1) by Bi2O3、WO3、TeO2Respectively in molar ratio 1:0.5:3 weigh ingredient, specifically weigh 3.9908 grams of Bi2O3、 1.9856 gram WO3, 9.0236 grams of TeO2, added raw materials into after mixing in nylon tank, ball milling 4~6 hours, embodiment 1-8 was specific Ball-milling Time is shown in Table 1；Raw material after ball milling is placed in infrared drying oven and dries, be sieved；
(2) it by the raw material after sieving, is calcined 3 hours in 400 DEG C；
(3) adding mass percent in powder after firing is that 5% PVA aqueous solution is granulated, and is sieved after drying, then The cylinder of Φ 12mm × 6mm is pressed into powder compressing machine；
(4) cylinder of step (3) is sintered in 480~530 DEG C, keeps the temperature 2~4 hours, embodiment 1-8 is specifically sintered temperature Degree and time are shown in Table 1, and Temperature Firing Microwave Dielectric Ceramics are made；
(5) microwave dielectric property of low-temperature sintered microwave dielectric ceramic material made from testing procedure (4).
See Table 1 for details for the test result of the related process parameters of embodiment 1-8 and microwave dielectric property.
The detection method of 1-8 of the embodiment of the present invention is as follows：
1, by Agilent 8720ES Network Analyzer, embodiment 1-8 is prepared using open type chamber parallel plate method Low-temperature sintered microwave dielectric ceramic material carry out dielectric constant measurement, by test fixture be put into high-low temperature chamber carry out resonance frequency The measurement of rate temperature coefficient, temperature range are 25-85 DEG C, and test frequency is within the scope of 6.8~7.6GHz.
2, the quality of low-temperature sintered microwave dielectric ceramic material being prepared using enclosed cell method measurement embodiment 1-8 because Number, test frequency is within the scope of 7.3~8.6GHz.
Table 1

Claims (8)

1. a kind of low-temperature sintered microwave dielectric ceramic material, it is characterised in that：Chemical composition is BiW0.5Te3O12。
2. a kind of preparation method of low-temperature sintered microwave dielectric ceramic material described in claim 1, it is characterised in that：Including such as Lower step：
(1) by raw material Bi2O3、WO3、TeO2BiW is pressed respectively0.5Te3O12Chemical formula weighs ingredient；
(2) all raw materials are mixed, is put into ball grinder, ball milling, by the raw material stoving after ball milling, sieving；
(3) powder for obtaining step (2) is calcined at 400 ± 10 DEG C；
(4) PVA aqueous solution is added in step (3) calcined powder to be granulated, is sieved after drying, then use powder compressing machine It is pressed into cylinder；
(5) cylinder for obtaining step (4) is sintered in 480~530 DEG C, and low-temperature sintered microwave dielectric ceramic material is made in heat preservation.
3. the preparation method of low-temperature sintered microwave dielectric ceramic material according to claim 2, it is characterised in that：Step (2) in Ball-milling Time be 4~6 hours, be sieved for 80 meshes.
4. the preparation method of low-temperature sintered microwave dielectric ceramic material according to claim 2, it is characterised in that：Step (3) calcination time is 3 ± 0.1 hours in.
5. the preparation method of low-temperature sintered microwave dielectric ceramic material according to claim 2, it is characterised in that：Step (4) PVA aqueous solution is the PVA aqueous solution that mass fraction is 5% in.
6. the preparation method of low-temperature sintered microwave dielectric ceramic material according to claim 2, it is characterised in that：Step (4) the cylindrical cylinder for being Φ 12mm × 6mm in.
7. the preparation method of low-temperature sintered microwave dielectric ceramic material according to claim 2, it is characterised in that：Step (4) pressure of powder compressing machine is 8~12MPa in.
8. the preparation method of low-temperature sintered microwave dielectric ceramic material according to claim 2, it is characterised in that：Step (5) soaking time is 2~4 hours in.
CN201810812107.4A 2018-07-23 2018-07-23 Low-temperature sintered microwave dielectric ceramic material and preparation method thereof Active CN108840666B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101747059A (en) * 2009-12-22 2010-06-23 上海大学 Method for preparing low temperature co-fired microwave dielectric ceramic material
CN103496981A (en) * 2013-09-26 2014-01-08 桂林理工大学 Low-temperature sintering temperature-stable microwave dielectric ceramic Bi14W2O27 and preparation method thereof
CN104671782A (en) * 2015-02-04 2015-06-03 桂林理工大学 Low-loss ultralow dielectric constant microwave dielectric ceramic Bi2WO6

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101747059A (en) * 2009-12-22 2010-06-23 上海大学 Method for preparing low temperature co-fired microwave dielectric ceramic material
CN103496981A (en) * 2013-09-26 2014-01-08 桂林理工大学 Low-temperature sintering temperature-stable microwave dielectric ceramic Bi14W2O27 and preparation method thereof
CN104671782A (en) * 2015-02-04 2015-06-03 桂林理工大学 Low-loss ultralow dielectric constant microwave dielectric ceramic Bi2WO6

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
姜善涛: "Bi2O3-TeO2系微波介质陶瓷烧结及其性能研究", 《兵器材料科学与工程》 *
张高群等: "超低温烧结微波介质陶瓷研究进展", 《硅酸盐学报》 *

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