CN104311037B - Ultralow dielectric microwave dielectric ceramic AlSi3v3n10and preparation method thereof - Google Patents

Ultralow dielectric microwave dielectric ceramic AlSi3v3n10and preparation method thereof Download PDF

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CN104311037B
CN104311037B CN201410565671.2A CN201410565671A CN104311037B CN 104311037 B CN104311037 B CN 104311037B CN 201410565671 A CN201410565671 A CN 201410565671A CN 104311037 B CN104311037 B CN 104311037B
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microwave
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dielectric ceramic
alsi
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CN104311037A (en
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陈进武
唐莹
苏和平
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Linquan Extraordinary Advertising Media Co ltd
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Guilin University of Technology
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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
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    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38Non-oxide ceramic constituents or additives
    • C04B2235/3852Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
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    • C04B2235/38Non-oxide ceramic constituents or additives
    • C04B2235/3852Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
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    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38Non-oxide ceramic constituents or additives
    • C04B2235/3852Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
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Abstract

The invention discloses a kind of ultralow dielectric microwave dielectric ceramic AlSi3V3N10And preparation method thereof.(1) be 99.9%(percentage by weight by purity) more than AlN, Si3N4And V3N5Starting powder press AlSi3V3N10Composition weigh dispensing;(2) by step (1) raw material wet ball-milling mix 12 hours, ball-milling medium is absolute ethyl alcohol, after drying in 1200 DEG C of nitrogen atmospheres pre-burning 6 hours;(3) the re-compacted shaping of powder prepared in step (2), finally sinters 8 hours in 1350 ~ 1400 DEG C of nitrogen atmospheres.Pottery prepared by the present invention is good at sintering, and dielectric constant reaches 5.2~5.7, and its quality factor q f value is up to 131000-162000GHz, and temperature coefficient of resonance frequency is little, industrially has great using value.

Description

Ultralow dielectric microwave dielectric ceramic AlSi3V3N10And preparation method thereof
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, telstar recipient 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 permittivity εr To adapt to different frequency and the requirement of different application occasion;(2) high quality factor q value or dielectric loss tan δ make an uproar to reduce Sound, typically requires Qf >=3000 GHz;(3) the temperature coefficient τ of resonant frequencyƒThe least to ensure the heat that device has had Stability, general requirement-10 ppm/DEG C≤τƒ≤+10 ppm/℃.Just have tried to from late 1930s in the world by Dielectric substance is applied to microwave technology, and prepares TiO2Microwave dielectric filter, but its temperature coefficient of resonance frequency τƒToo Greatly cannot be practical.Since the seventies in last century, start the large-scale development to medium ceramic material, according to Relative dielectric constant εrSize different from use frequency range, generally can have been developed that and the microwave-medium ceramics developed It 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.
Three performance indications (ε due to 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, electronic component With material, phase March the 3rd in 2005), meet three performance requirements and the single-phase microwave-medium ceramics of low temperature sintering is considerably less, Mainly their temperature coefficient of resonance frequency is the most excessive or quality factor are on the low side and cannot application request.The most right The research major part of microwave-medium ceramics is the summary of experience drawn by great many of experiments, does not but have complete theory to illustrate Microstructure and the relation of dielectric properties, therefore, the most also cannot predict its resonance from the composition of compound with structure The microwave dielectric property such as frequency-temperature coefficient and quality factor, which greatly limits microwave-medium ceramics and device Development.
Summary of the invention
It is an object of the invention to provide and a kind of there is good heat endurance and low-loss ultralow dielectric microwave be situated between Electroceramics material and preparation method thereof.
The chemical composition of the microwave dielectric ceramic material of the present invention is AlSi3V3N10
The preparation method step of this microwave dielectric ceramic material is:
(1) be 99.9%(percentage by weight by purity) more than AlN, Si3N4And V3N5Starting powder press AlSi3V3N10 Composition weigh dispensing.
(2) being mixed 12 hours by step (1) raw material wet ball-milling, ball-milling medium is absolute ethyl alcohol, at 1200 DEG C after drying Pre-burning 6 hours in nitrogen atmosphere.
(3) the re-compacted shaping of powder prepared in step (2), finally sinters 8 little in 1350 ~ 1400 DEG C of nitrogen atmospheres Time.
Advantages of the present invention: AlSi3V3N10Ceramic dielectric constant reaches 5.2~5.7, the temperature coefficient τ of its resonant frequencyƒ Little, temperature stability is good;Quality factor q f value is up to 131000-162000GHz, can be widely used for various medium substrate, resonance The manufacture of the microwave device such as device and wave filter, can meet the technology needs of low temperature co-fired technology and microwave multilayer device, in industry On have great using value.
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 system Preparation 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 nitride microwave dielectric ceramic, it is characterised in that described microwave dielectric ceramic Chemical composition be: AlSi3V3N10
The preparation method of described microwave dielectric ceramic concretely comprises the following steps:
(1) be 99.9%(percentage by weight by purity) more than AlN, Si3N4And V3N5Starting powder press AlSi3V3N10Group Become to weigh dispensing;
(2) being mixed 12 hours by step (1) raw material wet ball-milling, ball-milling medium is absolute ethyl alcohol, at 1200 DEG C of nitrogen after drying Pre-burning 6 hours in atmosphere;
(3) the re-compacted shaping of powder prepared in step (2), finally sinters 8 hours in 1350 ~ 1400 DEG C of nitrogen atmospheres.
CN201410565671.2A 2014-10-22 2014-10-22 Ultralow dielectric microwave dielectric ceramic AlSi3v3n10and preparation method thereof Expired - Fee Related CN104311037B (en)

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CN105236990A (en) * 2015-10-18 2016-01-13 桂林理工大学 Ultralow dielectric constant microwave dielectric ceramic LaNbB2O7 and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103130496A (en) * 2013-03-25 2013-06-05 桂林理工大学 Low-dielectric-constant microwave dielectric ceramic LiAlSi2O6 and preparation method thereof
CN103964835A (en) * 2014-04-27 2014-08-06 桂林理工大学 Temperature-stable microwave dielectric ceramic LiVP2O8 capable of being sintered at low temperature, and preparation method of ceramic

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103130496A (en) * 2013-03-25 2013-06-05 桂林理工大学 Low-dielectric-constant microwave dielectric ceramic LiAlSi2O6 and preparation method thereof
CN103964835A (en) * 2014-04-27 2014-08-06 桂林理工大学 Temperature-stable microwave dielectric ceramic LiVP2O8 capable of being sintered at low temperature, and preparation method of ceramic

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