CN106116522A - Temperature-stable ultralow dielectric microwave dielectric ceramic Mg3li2b2o7and preparation method thereof - Google Patents

Temperature-stable ultralow dielectric microwave dielectric ceramic Mg3li2b2o7and preparation method thereof Download PDF

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CN106116522A
CN106116522A CN201610434385.1A CN201610434385A CN106116522A CN 106116522 A CN106116522 A CN 106116522A CN 201610434385 A CN201610434385 A CN 201610434385A CN 106116522 A CN106116522 A CN 106116522A
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microwave
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dielectric ceramic
powder
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段炼
方亮
苏和平
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Guilin University of Technology
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Guilin University of Technology
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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
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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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    • 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
    • C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
    • C04B2235/3203—Lithium oxide 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
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206—Magnesium 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
    • C04B2235/34—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

Abstract

The invention discloses a kind of low temperature sintering temperature-stable ultralow dielectric microwave dielectric ceramic Mg3Li2B2O7And preparation method thereof.(1) be 99.9%(percentage by weight by purity) more than MgCO3、Li2CO3And H3BO3Starting powder press Mg3Li2B2O7Composition weigh dispensing；(2) by step (1) raw material wet ball-milling mix 12 hours, ball-milling medium is distilled water, after drying in 750 DEG C of air atmosphere pre-burning 6 hours；(3) after adding binding agent pelletize in the powder that step (2) prepares, re-compacted molding, finally sinter 4 hours in 800 ~ 840 DEG C of air atmosphere；Described binding agent uses mass concentration to be the poly-vinyl alcohol solution of 5%, and the addition of polyvinyl alcohol accounts for the 3% of powder gross mass.Pottery prepared by the present invention sinters well below 840 DEG C, and dielectric constant reaches 9.9～10.7, and its quality factor q f value is up to 89000 132000GHz, and temperature coefficient of resonance frequency is little, industrially has great using value.

Description

Temperature-stable ultralow dielectric microwave dielectric ceramic Mg3Li2B2O7And preparation Method
Technical field
The present invention relates to dielectric ceramic material, particularly relate to for manufacturing ceramic substrate, the resonance that microwave frequency uses Dielectric ceramic materials of microwave device such as device and wave filter and preparation method thereof.
Background technology
Microwave dielectric ceramic refers to be applied in microwave frequency band (mainly UHF and SHF frequency range) circuit as dielectric material And complete the pottery of one or more functions, modern communication is widely used as resonator, wave filter, dielectric substrate and medium The components and parts such as wave circuit, are the key foundation materials of modern communication technology, in portable mobile phone, automobile telephone, nothing The aspect such as rope phone, television satellite accepter and military radar has highly important application, small-sized at modern communication instrument Change, integrated during just playing increasing effect.
It is applied to the dielectric ceramic of microwave frequency band, should meet the requirement of following dielectric property: (1) seriation DIELECTRIC CONSTANT εr To adapt to different frequency and the requirement of different application occasion;(2) high quality factor q value or low dielectric loss tan δ are to reduce Noise, typically requires Qf >=3000 GHz;(3) the temperature coefficient τ of resonant frequencyƒThe least to ensure what device had had Heat stability, general requirement-10 ppm/DEG C≤τƒ≤+10 ppm/℃.Just have tried to from late 1930s in the world Dielectric substance is applied to microwave technology, and prepares TiO2Microwave dielectric filter, but its temperature coefficient of resonance frequency τƒ Too greatly cannot be practical.Since the seventies in last century, the large-scale development to medium ceramic material, root are started According to relative dielectric constant εrSize from use frequency range different, generally can will have been developed that and developing microwave-medium pottery Porcelain is divided into 4 classes.
(1) ultralow dielectric microwave dielectric ceramic, main representative is Al2O3-TiO2、Y2BaCuO5、MgAl2O4With Mg2SiO4Deng, its εr≤ 20, quality factor q × f >=50000GHz, τƒ≤10 ppm/°C.It is mainly used in microwave base plate and height End microwave device.
(2) low εrWith the microwave dielectric ceramic of high q-factor, mainly BaO-MgO-Ta2O5, BaO-ZnO-Ta2O5Or BaO- MgO-Nb2O5,BaO-ZnO-Nb2O5System or the hybrid system MWDC material between them.Its εr=20～35, Q=(1～2) × 104(under the GHz of f >=10), τƒ≈0.As medium in the microwave communication equipments such as the direct broadcasting satellite being mainly used in f >=8 GHz Resonating device.
(3) medium εrWith the microwave dielectric ceramic of Q-value, it is mainly with BaTi4O9、Ba2Ti9O20(Zr, Sn) TiO4Etc. for The MWDC material of base, its εr=35 ~ 45, Q=(6～9) × 103(under f=3～-4GHz), τƒ≤5 ppm/°C.It is mainly used in 4 ～8 in microwave military radar in GHz frequency range and communication system as dielectric resonance device.
(4) high εrAnd the microwave dielectric ceramic that Q-value is relatively low, in being mainly used in 0.8～4GHz frequency range, civilian movement is led to News system, this is also the emphasis of microwave dielectric ceramic research.Since the eighties, Kolar, Kato et al. in succession find and have studied Perovskite-like tungsten bronze type BaO Ln2O3—TiO2Series (Ln=La, Sm, Nd or Pr etc. are called for short BLT system), composite perofskite Structure C aO Li2O—Ln2O3—TiO2Series, lead base series material, Ca1-xLn2x/3TiO3It is contour εrMicrowave dielectric ceramic, The wherein BaO Nd of BLT system2O3—TiO2Material dielectric constant reaches 90, lead base series (Pb, Ca) ZrO3Dielectric constant reaches To 105.
The sintering temperature of the above material system is generally greater than 1300 ° of C, it is impossible to directly golden with the low melting point such as Ag and Cu Belong to burning altogether and form multilayer ceramic capacitor.In recent years, along with LTCC Technology (Low Temperature Co-fired Ceramics, LTCC) development and microwave multilayer device development requirement, research worker both domestic and external is to some low grade fever's systems Material has carried out exploring widely and studying, and mainly uses devitrified glass or glassceramic composites system, because of low melting point Glass has of a relatively high dielectric loss mutually, and the existence of glass phase substantially increases the dielectric loss of material.Therefore nothing is developed The low fired microwave dielectric ceramic material of glass phase is the emphasis of current research.
Explore novel with exploitation can be during low fired microwave dielectric ceramic materials, the Li base that intrinsic sintering temperature is low The material systems such as compound, Bi based compound, tungstates architecture compound and tellurate architecture compound get the attention with Research, but due to three performance indications (ε of microwave dielectric ceramicrWith Q f and τƒBetween) be mutually restriction relation (see Document: the restricting relation between microwave dielectric ceramic materials dielectric properties, Zhu Jianhua, Liang Fei, Wang little Hong, Lv Wenzhong, electronics unit Part and material, phase March the 3rd in 2005), satisfied three performance requirements and the single-phase microwave-medium ceramics of low temperature sintering are very Few, mainly their temperature coefficient of resonance frequency is the most excessive or quality factor are on the low side and cannot application request.Mesh The front research major part to microwave-medium ceramics is the summary of experience drawn by great many of experiments, does not but have complete theory Illustrate the relation of microstructure and dielectric properties, therefore, the most also cannot predict it from the composition of compound with structure The microwave dielectric property such as temperature coefficient of resonance frequency and quality factor, which greatly limits low temperature co-fired technology and micro- The development of ripple multilayer device.Explore with exploitation can low-temperature sintering have simultaneously near-zero resonance frequency temperature coefficient (-10 ppm/ ℃≤τƒ≤+10 ppm/ DEG C) with the microwave dielectric ceramic of higher figure of merit be those skilled in the art thirst for solving always but All the time the difficult problem succeeded it is difficult to.
Summary of the invention
It is an object of the invention to provide and a kind of have good heat stability and low-loss, low temperature sintering is ultralow simultaneously Dielectric constant microwave dielectric ceramic material and preparation method thereof.
The chemical composition of the microwave dielectric ceramic material of the present invention is Mg3Li2B2O7。
The preparation method step of this microwave dielectric ceramic material is:
(1) be 99.9%(percentage by weight by purity) more than MgCO3、Li2CO3And H3BO3Starting powder press Mg3Li2B2O7 Composition weigh dispensing.
(2) being mixed 12 hours by step (1) raw material wet ball-milling, ball-milling medium is distilled water, at 750 DEG C of air after drying Pre-burning 6 hours in atmosphere.
(3), after adding binding agent pelletize in the powder that step (2) prepares, re-compacted molding, finally at 800 ~ 840 DEG C Air atmosphere sinters 4 hours；Described binding agent uses mass concentration to be the poly-vinyl alcohol solution of 5%, polyvinyl alcohol addition Account for the 3% of powder gross mass.
Advantages of the present invention: Mg3Li2B2O7Ceramic sintering temperature is low, and cost of material is low；Its quality factor q f value is up to 89000-132000GHz, dielectric constant reaches 9.9～10.7, the temperature coefficient τ of its resonant frequencyƒLittle, temperature stability is good； Can be widely used for the manufacture of the microwave devices such as various medium substrate, resonator and wave filter, low temperature co-fired technology and micro-can be met The technology of ripple multilayer device needs.
Detailed description of the invention
Embodiment:
Table 1 shows 3 specific embodiments and the microwave dielectric property thereof of the different sintering temperatures constituting the present invention.Its preparation side Method as it has been described above, carry out the evaluation of microwave dielectric property by cylindrical dielectric resonator method.
This pottery can be widely used for the manufacture of the microwave devices such as various medium substrate, resonator and wave filter, can meet shifting The technology of the systems such as dynamic communication and satellite communication needs.
Table 1:

Claims (1)

1. a temperature-stable ultralow dielectric microwave dielectric ceramic, it is characterised in that described ultralow dielectric microwave is situated between The chemical composition of electroceramics is: Mg3Li2B2O7；
The preparation method of described ultralow dielectric microwave dielectric ceramic concretely comprises the following steps:
(1) be 99.9%(percentage by weight by purity) more than MgCO3、Li2CO3And H3BO3Starting powder press Mg3Li2B2O7 Composition weigh dispensing；
(2) being mixed 12 hours by step (1) raw material wet ball-milling, ball-milling medium is distilled water, 750 DEG C of air atmosphere after drying Middle pre-burning 6 hours；
(3), after adding binding agent pelletize in the powder that step (2) prepares, re-compacted molding, finally at 800 ~ 840 DEG C of air Atmosphere sinters 4 hours；Described binding agent uses mass concentration to be the poly-vinyl alcohol solution of 5%, and polyvinyl alcohol addition accounts for powder The 3% of end gross mass.
CN201610434385.1A 2016-06-19 2016-06-19 Temperature-stable ultralow dielectric microwave dielectric ceramic Mg3li2b2o7and preparation method thereof Pending CN106116522A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110041067A (en) * 2019-04-19 2019-07-23 贵阳顺络迅达电子有限公司 A kind of low high Q temperature-stable perovskite structure LTCC microwave dielectric material and preparation method thereof that is situated between

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1524792A (en) * 2003-02-28 2004-09-01 新加坡纳米材料科技有限公司 Method for preparing crystalline state perovskite compounds powder
CN104496422A (en) * 2014-12-02 2015-04-08 桂林理工大学 Low-temperature sintered temperature-stable microwave dielectric ceramic Li3Mg2BO5 and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1524792A (en) * 2003-02-28 2004-09-01 新加坡纳米材料科技有限公司 Method for preparing crystalline state perovskite compounds powder
CN104496422A (en) * 2014-12-02 2015-04-08 桂林理工大学 Low-temperature sintered temperature-stable microwave dielectric ceramic Li3Mg2BO5 and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110041067A (en) * 2019-04-19 2019-07-23 贵阳顺络迅达电子有限公司 A kind of low high Q temperature-stable perovskite structure LTCC microwave dielectric material and preparation method thereof that is situated between
CN110041067B (en) * 2019-04-19 2021-12-28 贵阳顺络迅达电子有限公司 Low-dielectric high-Q temperature-stable type perovskite structure LTCC microwave dielectric material and preparation method thereof

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