CN110256088A - A kind of microwave-medium ceramics composite sintering agent and preparation method thereof - Google Patents
A kind of microwave-medium ceramics composite sintering agent and preparation method thereof Download PDFInfo
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- CN110256088A CN110256088A CN201910516282.3A CN201910516282A CN110256088A CN 110256088 A CN110256088 A CN 110256088A CN 201910516282 A CN201910516282 A CN 201910516282A CN 110256088 A CN110256088 A CN 110256088A
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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
- C04B35/6303—Inorganic additives
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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
- C04B2235/3215—Barium oxides or oxide-forming salts thereof
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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
- C04B2235/3281—Copper oxides, cuprates or oxide-forming salts thereof, e.g. CuO or Cu2O
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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
- C04B2235/34—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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Abstract
The invention discloses a kind of microwave-medium ceramics composite sintering agents and preparation method thereof, belong to electronic information function material and device arts.The present invention is formed by main component of barium copper boron compound to be prepared using solid reaction process, and the sintering aid for the microwave-medium ceramics that can be used in LTCC technique reduces the sintering temperature of microwave-medium ceramics, meets the requirement of LTCC technique, without deteriorating dielectric properties.Material of the present invention can adjust dielectric properties, it can be achieved that stablizing dielectric properties in wide temperature range by changing process conditions.Sintering aid material of the invention has the characteristics that stability is good, consistency is good, reproducible, suitable for reducing the microwave-medium ceramics sintering temperature LTCC, meets the requirement of LTCC technique.
Description
Technical field
The invention belongs to electronic information function material and device arts, and in particular to be a kind of microwave-medium ceramics
Composite sintering agent and preparation method thereof.The sintering aid for the microwave-medium ceramics that can be used in LTCC technique reduces microwave-medium
The sintering temperature of ceramics meets the requirement of LTCC technique, without deteriorating dielectric properties.
Background technique
In recent years, mobile communication and portable terminal are just sent out towards miniaturization, lightweight, integrated and inexpensive direction
Exhibition, to microwave device, higher requirements are also raised for this.To meet this requirement, exploitation low-temperature co-burning ceramic material (LTCC) at
For hot spot.Consider that microwave-medium ceramics can be with lower melting-point Ag (961 DEG C) or Cu (1 064 from economy and feature of environmental protection angle
DEG C) electrode material carry out it is low temperature co-fired then ideal.
In terms of current existing research work, realizes that the low sintering technological approaches of microwave-medium ceramics mainly has: (1) selecting
Select the low material of intrinsic sintering temperature；(2) it is synthesized using wet chemical methods and the ultra-fine powder raw material of selection, by tiny powder
The high-ratio surface of body, high activity improve sintering driving force, to reduce sintering temperature；(3) selection low melting point sintering aid comes
Reduce sintering temperature.Wherein, addition low melting point sintering aid is most widely used come the sintering temperature for reducing material.
Therefore there is an urgent need to develop suitable sintering aids.
BaCu(B2O5) (BCB) ceramics have low melting point (about 850 DEG C) and excellent microwave dielectric property (r=7.4 ε,
Qf=50 000 GHz, τf= –32×10–6/ DEG C), as low melting point sintering aid, successfully by the burning of a variety of ceramics
Junction temperature drops to 950 DEG C hereinafter, such as BaSm2Ti4012、Ba(znl/3 Nb2/3)03、Ba3Ti5Nb6O28、Ba5Nb4O15-
BaWO4、CaO-Li2O-Sm2O3-TiO2And BaTi4O9Etc. each series microwave dielectric ceramic.
Summary of the invention
That the object of the present invention is to provide a kind of consistency is good, the microwave-medium ceramics sintering aid stably produced can be achieved
And preparation method thereof.
Primary focus of the invention is that the technique of microwave-medium ceramics sintering aid determines, can root in actual application
According to needing to adjust accordingly synthetic method and production technology, flexibility is big.Grinding aid selects dehydrated alcohol, speed when dry
Fastly, it is not easy to cause segregation to be layered and make raw material mixing uneven, and dried pieces hardness is small, is easy to crush.The present invention selects suitable
In the solid reaction process of industrial mass production, being conducive to production cost is reduced.
The present invention solve the technical problem the technical solution adopted is as follows:
The structural formula of the sintering aid of microwave-medium ceramics of the invention are as follows: BaCu (B205), in formula components containing barium, copper,
Boron element, raw material Ba, Cu, the B for preparing this material can be oxide, inorganic salts containing these elements.
A kind of microwave-medium ceramics composite sintering agent, by main crystal phase material through ball milling mixing, pre-burning, filters pressing drying, crushing
It is made；Wherein: the main crystal phase material is Ba (OH)2·8H2O mass percent is that 60.9%, CuO mass percent is
15.3%, H3BO3Mass percent is 23.8%.
Molar ratio in the main crystal phase material between Ba, Cu, B is 1: 1: 2.
A kind of preparation method of microwave-medium ceramics composite sintering agent, feature include the following steps: (1), principal crystalline phase material
Material preparation weighs Ba (OH) in molar ratio at 1: 1: 22·8H2O、CuO、H3BO3, in material: ball: the ratio 2.5: 1 of dehydrated alcohol:
1.5 carry out ball milling, after drying, pre-burning under the conditions of 860/6H.
(2), the main crystal phase material after pre-burning, in material after crushing: ball: the ratio 2.5: 1: 1.5 of dehydrated alcohol carries out ball milling,
Drying, then pulverizes and sieves.
The detection of microwave-medium ceramics sintering aid of the invention is using coating silver paste, and high temperature burning infiltration is electrode, measurement member
The dielectric properties of part.
The characteristic and Heterosis of microwave-medium ceramics sintering aid of the present invention exist: 1. material composition is simple, former material
Material is relatively abundanter, environmental-friendly；2. sintering temperature is lower in preparation process, production cost is reduced；3. material is made with dehydrated alcohol
For grinding aid.
The electrical property of microwave-medium ceramics sintering aid of the present invention can realize following parameter request: dielectric constant=7.4, damage
Consume the GHz of factor Qf=50 000, temperature coefficient of resonance frequency τf= –32×10–6 /℃。
The contents of the present invention are further described with the following Examples.Following embodiment only meets the technology of the present invention
Several examples of content do not illustrate that present invention is limited only to contents described in following examples.Of the invention focuses on technique side
Method.
Specific embodiment
The present invention uses the Ba (OH) of purity assay2·8H2O、CuO、H3BO3Principal crystalline phase, specific embodiment party are prepared for raw material
Formula is as follows: pressing Ba (OH)2·8H2O、CuO、H3BO3Molar ratio 1:1:2 weighs ingredient, and mixture is put into stirring-type ball grinder
In, by ball: material: dehydrated alcohol mass ratio 2.5:1:1.5, ball milling 10 ± 2 hours, revolving speed was 280 revs/min.Granularity control
In D50Within=1.5 μm, by the material filters pressing that ball milling is mixed, 80 DEG C of baking oven drying is put in, 40 meshes are smashed it through, in box resistance
860 DEG C/6H condition pre-burning is pressed in furnace, and it is spare to smash it through 40 meshes；By ball: material: the ratio of dehydrated alcohol mass ratio 2.5:1:0.5
Example carries out secondary ball milling, filters pressing, drying, D50Within=1.2 μm, 80 meshes are smashed it through, PVA is added to be granulated, use handpress
20MPa forms Φ 12.2mm × 2mm disk.Green compact sample is placed in sintering furnace, under the conditions of 860 DEG C/4H, sinters Ceramic Like into
Product, Tu Yinhou burning infiltration under the conditions of 820 DEG C/10M carry out performance survey to sample by impedance analyzer 4291B, micrometer etc.
Examination.
The specific embodiment of the invention is shown in Table 1 at porcelain density, dielectric constant, loss factor, temperature coefficient result in detail.
The condition and properties of sample of each example of table 1
Claims (3)
1. a kind of microwave-medium ceramics composite sintering agent, it is characterised in that dried by main crystal phase material through ball milling mixing, pre-burning, filters pressing
Dry, crushing is made；Wherein: the main crystal phase material is Ba (OH)2·8H2O mass percent is 60.9%, CuO mass percentage
Than for 15.3%, H3BO3Mass percent is 23.8%.
2. a kind of microwave-medium ceramics composite sintering agent according to claim 1, it is characterised in that the main crystal phase material
Molar ratio between middle Ba, Cu, B is 1: 1: 2.
3. a kind of preparation method of microwave-medium ceramics composite sintering agent, feature includes the following steps: prepared by main crystal phase material,
Weigh Ba (OH) at 1: 1: 2 in molar ratio2·8H2O、CuO、H3BO3, in material: ball: the ratio 2.5: 1: 1.5 of dehydrated alcohol carries out ball
Mill, after drying, pre-burning under the conditions of 860/6H；Main crystal phase material after pre-burning, in material after crushing: ball: the ratio of dehydrated alcohol
Carry out ball milling at 2.5: 1: 1.5, then drying pulverizes and sieves.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112750551A (en) * | 2019-10-31 | 2021-05-04 | 东莞华科电子有限公司 | Electrode paste, electrode, ceramic electronic component including the same, and method of manufacturing the component |
| CN114394828A (en) * | 2022-01-10 | 2022-04-26 | 湖南省美程陶瓷科技有限公司 | Electronic ceramic material with medium dielectric constant and preparation method thereof |
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| US20090033441A1 (en) * | 2005-03-31 | 2009-02-05 | Matsushita Electric Industrial Co., Ltd. | Dielectric porcelain composition and high frequency device using the same |
| CN101486569A (en) * | 2009-02-24 | 2009-07-22 | 同济大学 | Low temperature sintering microwave ceramic material and preparation thereof |
| CN101613200A (en) * | 2009-07-21 | 2009-12-30 | 西安交通大学 | A kind of low-temperature sintered microwave dielectric ceramic material and preparation method thereof |
| CN101792319A (en) * | 2010-04-07 | 2010-08-04 | 陕西科技大学 | Preparation method of low temperature sintered magnetoelectric composite ceramic material |
| CN104556996A (en) * | 2015-01-14 | 2015-04-29 | 陕西科技大学 | BaFe12O19/CoFe2O4 permanent-magnet composite ceramic material and preparation method thereof |
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2019
- 2019-06-14 CN CN201910516282.3A patent/CN110256088A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090033441A1 (en) * | 2005-03-31 | 2009-02-05 | Matsushita Electric Industrial Co., Ltd. | Dielectric porcelain composition and high frequency device using the same |
| CN101486569A (en) * | 2009-02-24 | 2009-07-22 | 同济大学 | Low temperature sintering microwave ceramic material and preparation thereof |
| CN101613200A (en) * | 2009-07-21 | 2009-12-30 | 西安交通大学 | A kind of low-temperature sintered microwave dielectric ceramic material and preparation method thereof |
| CN101792319A (en) * | 2010-04-07 | 2010-08-04 | 陕西科技大学 | Preparation method of low temperature sintered magnetoelectric composite ceramic material |
| CN104556996A (en) * | 2015-01-14 | 2015-04-29 | 陕西科技大学 | BaFe12O19/CoFe2O4 permanent-magnet composite ceramic material and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112750551A (en) * | 2019-10-31 | 2021-05-04 | 东莞华科电子有限公司 | Electrode paste, electrode, ceramic electronic component including the same, and method of manufacturing the component |
| CN112750551B (en) * | 2019-10-31 | 2022-10-18 | 东莞华科电子有限公司 | Electrode paste, electrode, ceramic electronic component including the same, and method of manufacturing the component |
| CN114394828A (en) * | 2022-01-10 | 2022-04-26 | 湖南省美程陶瓷科技有限公司 | Electronic ceramic material with medium dielectric constant and preparation method thereof |
| CN114394828B (en) * | 2022-01-10 | 2022-10-18 | 湖南省美程陶瓷科技有限公司 | Electronic ceramic material with medium dielectric constant and preparation method thereof |
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Application publication date: 20190920 |