CN107399966A - Low dielectric microwave dielectric material of a kind of high-performance and preparation method thereof - Google Patents

Low dielectric microwave dielectric material of a kind of high-performance and preparation method thereof Download PDF

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CN107399966A
CN107399966A CN201710629131.XA CN201710629131A CN107399966A CN 107399966 A CN107399966 A CN 107399966A CN 201710629131 A CN201710629131 A CN 201710629131A CN 107399966 A CN107399966 A CN 107399966A
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dielectric material
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microwave dielectric
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黄新友
高春华
李军
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Jiangsu University
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Abstract

The present invention relates to technical field of inorganic nonmetallic materials, refers in particular to low dielectric microwave dielectric material of a kind of high-performance and preparation method thereof.The formula of the dielectric material includes in terms of weight percentage:ZnAl2O460 92%, TiO24 25%, MgO 1 10%, Cr2O30.01 1.5%, CeO20.01 1%, LaNiO30.5 3%, Sr3Cu Nb2O90.5 4%.The microwave dielectric material dielectric constant is 10~13, has the characteristics of high quality factor, low frequency temperature coefficient.

Description

Low dielectric microwave dielectric material of a kind of high-performance and preparation method thereof
Technical field
The present invention relates to technical field of inorganic nonmetallic materials, refers in particular to a kind of microwave dielectric material;It uses microwave-medium Material preparation method, using the general chemistry raw material of microwave dielectric material, be prepared high q-factor, low frequency temperature coefficient it is micro- Ripple dielectric material, to meet the requirement in present mobile communication application to microwave dielectric material high q-factor and low frequency temperature coefficient, Application especially in terms of the cavity microwave device such as coated by dielectric metal cavity filter and duplexer.
Background technology
Microwave-medium ceramics (MWDC), refer to be applied to be used as dielectric material in microwave frequency band circuit and complete a kind of or more The ceramics of kind function, are widely used in the communication systems such as satellite television, radar, mobile communication, mobile device in modern communication The various fields such as system and modern medicine.
With forth generation radio communication, i.e. 4G development, to key foundation material --- the microwave in modern communications technology The requirement more and more higher of medium ceramic material, is requiring permittivity εrTowards the development of higher and ultralow both direction, frequency temperature Spend coefficient τfWhile as small as possible, also require that quality factor (Q) are as high as possible to meet the design application in different communication field It is required that;But quality factor (Q) value and frequency-temperature coefficient of current microwave dielectric material are not felt quite pleased also, up for changing Kind, therefore, exploitation high quality factor (Q) value, low frequency temperature coefficient are the developing direction of microwave dielectric material.
The present invention is exactly to succeed in developing under this background, to meet in present mobile communication application to material high-quality The requirement of factor value and low frequency temperature coefficient, especially in the cavity microwave device such as coated by dielectric metal cavity filter and duplexer Application in terms of part.
The content of the invention
It is an object of the invention to provide a kind of matching somebody with somebody for the microwave dielectric material of high quality factor value and low frequency temperature coefficient Side and preparation technology.
The object of the present invention is achieved like this:
The medium formula includes in terms of weight percentage:ZnAl2O460-92%, TiO24-25%, MgO 1- 10%, Cr2O30.01-1.5%, CeO20.01-1%, LaNiO30.5-3%, Sr3CuNb2O90.5-4%.
Wherein ZnAl2O4、LaNiO3、Sr3CuNb2O9It is to use conventional chemical raw material with Solid phase synthesis respectively.
ZnAl used in the ceramic material of the present invention2O4Preparation process include:By routine chemical raw material ZnO and Al2O3By 1:1 molar ratio ingredient, it is put into after ground and mixed is uniform in alumina crucible and is incubated 120 minutes in 1150 DEG C, solid phase is anti- ZnAl should be synthesized2O4, ground 200 mesh sieve, standby after cooling.
LaNiO used in the ceramic material of the present invention3Preparation process include:By the chemical raw material La of routine2O3、 Ni2O3By 1/2:1/2 molar ratio ingredient, it is put into after ground and mixed is uniform in alumina crucible and is incubated 120 minutes in 1150 DEG C, Gu Phase reaction synthesizes LaNiO3, ground 200 mesh sieve, standby after cooling.
Sr used in the ceramic material of the present invention3CuNb2O9Preparation process include:By the chemical raw material of routine SrCO3, CuO and Nb2O5By 3:1:1 molar ratio ingredient, it is put into after ground and mixed is uniform in alumina crucible in 1280 DEG C of insulations 120 minutes, solid state reaction kinetics Sr3CuNb2O9, ground 200 mesh sieve, standby after cooling.
The ceramic material of the present invention is prepared using following technique:Dispensing, precise are carried out according to the formula of dielectric material Various raw materials are simultaneously poured into ball grinder, add deionized water and ZrO2Abrading-ball, then it is put into ball milling on planetary ball mill, 300r/ Slurry, is put into baking oven by min rotating speeds continuous ball milling 6 hours after discharging, is dried at 80~120 DEG C;Crushed after drying, then 60 mesh sieves are crossed, obtain even-grained powder;14~17% concentration that powder weight is added in powder is the poly- of 10wt% Alcohol adhesive, it is granulated, after being ground uniformly in mortar, the feed powder of the mesh granularity of 60 mesh~120 is taken, in 130Mpa pressure Under it is dry-pressing formed;2 hours are incubated with dumping at 500 DEG C after shaping, then with 3 DEG C/min heating rate, 1280~1320 DEG C insulation sinters for 3 hours, final obtained dielectric constant 10~13, high quality factor (Q) value, low frequency temperature coefficient it is new Microwave dielectric material.
The advantages of present media material is:Dielectric constant (ε can be obtainedr) it is 10~13, frequency-temperature coefficient (τf) < The novel microwave dielectric material of ± 2ppm/ DEG C (- 45~25 DEG C or 25~+85 DEG C), high quality factor (Q is 13810~13860) Material, a brand-new material foundation is provided for the exploitation of high performance microwave device.
Embodiment
According to material side's ratio range of above-mentioned microwave dielectric material, the dielectric material formula of specific embodiment is as shown in table 1.
The formula of the embodiments of the invention of table 1 totally 5 samples
According to above-mentioned material formula, the various raw materials of precise are simultaneously poured into resin ball grinder, add deionized water and ZrO2Abrading-ball, material/water/ball=1:3:1 (weight), then it is put into ball milling on planetary ball mill, 300r/min rotating speeds continuous ball milling 6 Hour, slurry is put into baking oven after discharging, dried at 80~120 DEG C.Crushed after drying, then cross 60 mesh sieves, obtain grain Spend uniform powder;14~17% concentration that powder weight is added in powder is 10wt% poly (vinyl alcohol) binder, is entered Row is granulated, and after being ground uniformly in mortar, takes the feed powder of the mesh granularity of 60 mesh~120, dry-pressing formed under 130Mpa pressure;Simultaneously Make two kinds of samples:TE01 δ moulds resonator (height H is about diameter D half) material sample and DR resonators (4 × 4mm Resonator) use material sample;2 hours are incubated so as to abundant dumping at 500 DEG C after shaping, then with 3 DEG C/min heating rate, Sintered within 3 hours in 1280~1320 DEG C of insulations, after coming out of the stove, given size is ground to according to test request, with Agilent E5071B Network Analyzer tests microwave dielectric property under 6.95GHz frequency.
Method of testing:
1. with parallel shorts plate method (Hakki-Coleman), micro-wave dielectric is tested with Agilent E5071B Network Analyzers Performance.
2. its frequency-temperature coefficient (τ is tested in high-low temperature test chamber with the resonator of DR4 × 4f), Range of measuring temp For -45~25 DEG C or 25 DEG C~+85 DEG C.
3. utilize the density (ρ) of Archimedes principle drainage test sample product.
Test result:Performance test is carried out to the sample of above-described embodiment, test result is as shown in table 2.
The dielectric constant of prepared microwave dielectric material is 10~13 as can be seen from Table 2, and high quality factor (Q) are 13810~13860, low frequency-temperature coefficient (τf) < ± 2ppm/ DEG C (- 45~25 DEG C or 25~+85 DEG C).
The performance of the Example formulations sample of table 2
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention All any modification, equivalent and improvement made within refreshing and principle etc., should be included in the scope of the protection.

Claims (6)

  1. A kind of 1. low dielectric microwave dielectric material of high-performance, it is characterised in that:The dielectric material formula, according to percentage by weight table Show including:ZnAl2O460-92%, TiO24-25%, MgO 1-10%, Cr2O30.01-1.5%, CeO20.01-1%, LaNiO30.5-3%, Sr3CuNb2O90.5-4%, wherein ZnAl2O4、LaNiO3、Sr3CuNb2O9It is using routine respectively Chemical raw material is with Solid phase synthesis.
  2. A kind of 2. low dielectric microwave dielectric material of high-performance as claimed in claim 1, it is characterised in that:Jie of the dielectric material Electric constant εrFor 10~13;Frequency-temperature coefficient τf< ± 2ppm/ DEG C, Range of measuring temp is -45~25 DEG C or 25 DEG C~+85 ℃;High quality factor Q is 13810~13860.
  3. A kind of 3. low dielectric microwave dielectric material of high-performance as claimed in claim 1, it is characterised in that described ZnAl2O4System Standby process includes:By the chemical raw material ZnO and Al of routine2O3By 1:1 molar ratio ingredient, aluminum oxide is put into after ground and mixed is uniform 120 minutes are incubated in 1150 DEG C in crucible, solid state reaction kinetics ZnAl2O4, ground 200 mesh sieve, standby after cooling.
  4. A kind of 4. low dielectric microwave dielectric material of high-performance as claimed in claim 1, it is characterised in that described LaNiO3System Standby process includes:By the chemical raw material La of routine2O3、Ni2O3By 1/2:1/2 molar ratio ingredient, oxygen is put into after ground and mixed is uniform Change in aluminium crucible and be incubated 120 minutes in 1150 DEG C, solid state reaction kinetics LaNiO3, ground 200 mesh sieve, standby after cooling.
  5. A kind of 5. low dielectric microwave dielectric material of high-performance as claimed in claim 1, it is characterised in that:Described Sr3CuNb2O9 Preparation process include:By the chemical raw material SrCO of routine3, CuO and Nb2O5By 3:1:1 molar ratio ingredient, ground and mixed are uniform After be put into alumina crucible and be incubated 120 minutes in 1280 DEG C, solid state reaction kinetics Sr3CuNb2O9, ground 200 mesh after cooling Sieve, it is standby.
  6. A kind of 6. preparation method of the low dielectric microwave dielectric material of high-performance as claimed in claim 1, it is characterised in that specific step It is rapid as follows:Dispensing is carried out according to the formula of dielectric material, the various raw materials of precise are simultaneously poured into ball grinder, add deionized water And ZrO2Abrading-ball, ball milling on planetary ball mill is then put into, 300r/min rotating speeds continuous ball milling 6 hours, is put slurry after discharging Enter in baking oven, dried at 80~120 DEG C;Crushed after drying, then cross 60 mesh sieves, obtain even-grained powder;In powder The poly (vinyl alcohol) binder that middle 14~17% concentration for adding powder weight is 10wt%, is granulated, is ground in mortar After uniformly, the feed powder of the mesh granularity of 60 mesh~120 is taken, it is dry-pressing formed under 130Mpa pressure;After shaping 2 hours are incubated at 500 DEG C With dumping, then with 3 DEG C/min heating rate, sintered within 3 hours in 1280~1320 DEG C of insulations, finally obtained dielectric constant exists 10~13, high quality factor (Q) value, the microwave dielectric material of low frequency temperature coefficient.
CN201710629131.XA 2017-07-28 2017-07-28 Low dielectric microwave dielectric material of a kind of high-performance and preparation method thereof Withdrawn CN107399966A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110845226A (en) * 2019-11-29 2020-02-28 杭州电子科技大学 Microwave dielectric ceramic material SrGa2O4And method for preparing the same

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104446442A (en) * 2014-11-28 2015-03-25 黄新友 Microwave medium material and preparation method thereof
CN104944937A (en) * 2015-06-15 2015-09-30 桂林理工大学 ZnAl2O4/Li4Ti5O12 microwave dielectric ceramic material and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104446442A (en) * 2014-11-28 2015-03-25 黄新友 Microwave medium material and preparation method thereof
CN104944937A (en) * 2015-06-15 2015-09-30 桂林理工大学 ZnAl2O4/Li4Ti5O12 microwave dielectric ceramic material and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
A. A. BUSH ETAL.: "Dielectric Properties of Sr3CuNb2O9 Perovskite Ceramics", 《INORGANIC MATERIALS》 *
K.P. SURENDRAN ETAL.: "Temperature stable low loss ceramic dielectrics in (1-x)ZnAl2O4-xTiO2 system for microwave substrate applications", 《THE EUROPEAN PHYSICAL JOURNAL B》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110845226A (en) * 2019-11-29 2020-02-28 杭州电子科技大学 Microwave dielectric ceramic material SrGa2O4And method for preparing the same

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Application publication date: 20171128