CN108314444A - A kind of high q-factor rock salt class microwave dielectric material - Google Patents

A kind of high q-factor rock salt class microwave dielectric material Download PDF

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CN108314444A
CN108314444A CN201810200792.5A CN201810200792A CN108314444A CN 108314444 A CN108314444 A CN 108314444A CN 201810200792 A CN201810200792 A CN 201810200792A CN 108314444 A CN108314444 A CN 108314444A
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microwave dielectric
rock salt
dielectric material
powder
salt class
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李玲霞
杜明昆
于仕辉
许振鹏
乔坚栗
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Tianjin University
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Tianjin University
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    • C04B35/465—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 based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates
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    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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Abstract

The invention discloses a kind of high q-factor rock salt class microwave dielectric materials, with MgO, TiO2、Al2O3、Nb2O5And Li2CO3For raw material, target synthetic expression formula is Li2Mg3Ti1‑x(Al1/2Nb1/2)xO6(0 x≤0.95 ＜).First stoichiometrically formula carries out dispensing, then in 900~1100 DEG C of pre-burnings after ball milling, drying, sieving, then is granulated, then pressure forming is green compact after drying, sieving, and high q-factor rock salt class Li is made in 1180 DEG C of 1340 DEG C of sintering in green compact2Mg3TiO6Base microwave dielectric material.Qf values of the present invention are up to 143,115~162,429GHz, and have lower dielectric loss, and preparation process is simple, while having both moderate εrValue 13.21~14.31 is with a wide range of applications by the microwave dielectric properties that it is fabricated to.

Description

A kind of high q-factor rock salt class microwave dielectric material
Technical field
The ceramic composition that the invention belongs to a kind of characterized by ingredient, more particularly to a kind of novel high q-factor rock salt class are micro- Wave dielectric material and preparation method thereof
Background technology
Microwave-medium ceramics have compact-sized, and light-weight, the features such as thermal stability is good, at low cost, function admirable, is nothing Indispensable component part in line communication.With the continuous development of wireless communication technique, more and more microwave devices use Dielectric resonator is situated between to dielectric resonator high q-factor (quality factor) dielectric constant microwave as its frequency determination part part The demand of material is growing.Because high q-factor (>100,000GHz) FREQUENCY CONTROL precision can be improved, is inhibited in circuit Electronic noise, low-k (<15) propagation delay time can be reduced, ensures the accuracy and promptness of signal.Cause This, the new material that searching meets all above-mentioned requirements is one of the significant challenge that electronics industry faces.
Some researches show that the Li with rock salt structure recently2Mg3TiO6Base microwave dielectric material, raw material is relatively cheap, system It is standby simple for process, but sintering temperature is relatively high (~1280 DEG C), it is less to the modified report of its microwave dielectric property.Cause This, passes through additive agent modified raising Li2Mg3TiO6Qf values, while reducing its sintering temperature to a certain extent, become current Urgent problem to be solved.
Invention content
The purpose of the present invention is the Li with rock salt structure to the prior art2Mg3TiO6Base microwave dielectric material introduces Additive A l2O3And Nb2O5, to improve Li2Mg3TiO6The Qf values of microwave dielectric material.Wherein, Al2O3Not only act as acceptor doping Effect, and be conducive to Ceramic grain growth and its uniformity, Nb2O5It is used for keeping charge as a kind of donor dopant Balance.Finally, provide a kind of high q-factor (>140,000GHz)Li2Mg3TiO6Base microwave dielectric material.
The present invention is achieved by following technical solution.
A kind of high q-factor rock salt class microwave dielectric material, with MgO, TiO2、Al2O3、Nb2O5And Li2CO3For raw material, by solid Prepared by phase method, target synthetic expression formula is Li2Mg3Ti1-x(Al1/2Nb1/2)xO6, wherein 0 x≤0.95 ＜.
The high q-factor rock salt class microwave dielectric material, specific implementation step are as follows：
(1) by MgO, TiO2、Al2O3、Nb2O5And Li2CO3Stoichiometrically formula Li2Mg3Ti1-x(Al1/2Nb1/2)xO6, wherein X=0~0.95 carries out dispensing, and powder is put into polyester ball grinder, after absolute ethyl alcohol and zirconia ball is added, ball milling 4~24 Hour；
(2) raw material after step (1) ball milling is put into drying box, in 100~120 DEG C of drying, then crosses 40 mesh sieve；
(3) powder after step (2) being sieved is put into alumina crucible and is built in moderate oven, pre- in 900~1100 DEG C It burns, keeps the temperature 2~8 hours, then cross 40 mesh sieve；
(4) the PVA powder that the powder additional mass percent content after step (3) being sieved is 0.7% mixes, and puts Enter in polyester ball grinder, after absolute ethyl alcohol and zirconia ball is added, ball milling is granulated for 4~24 hours；
(5) by step (4) be granulated after powder be put into drying box, in 100~120 DEG C dry 4~6 hours, then Cross 80 mesh sieve；
(6) green compact are made with the pressure of 4~8MPa with powder compressing machine in the powder of step (5)；
(7) green compact of step (6) are kept the temperature 2~8 hours, high q-factor rock salt class is made in 1180 DEG C of -1340 DEG C of sintering Li2Mg3TiO6Base microwave dielectric material.
The step (1), (4) are all made of planetary ball mill and carry out ball milling, and drum's speed of rotation is 400 revs/min.
The step (1), the raw material of (4) and the mass ratio of absolute ethyl alcohol and zirconia ball are 1:30:15.
The a diameter of 10mm of green compact of the step (6), thickness are 4~5mm.
The present invention is with MgO, TiO2、Al2O3、Nb2O5And Li2CO3Novel high q-factor rock salt class microwave-medium material is prepared for raw material Expect Li2Mg3Ti1-x(Al1/2Nb1/2)xO6(x=0~0.95).Under microwave frequency band, which measures Qf under optimal sintering temperature Value is up to 143,115~162,429GHz, and has lower dielectric loss.Ceramic systems preparation process is simple, simultaneously Have both moderate εrValue 13.21~14.31 is with a wide range of applications by the microwave dielectric properties that it is fabricated to.
Specific implementation mode
The present invention is more than 99% MgO, TiO with purity2、Al2O3、Nb2O5And Li2CO3For initial feed, pass through solid phase method Prepare microwave dielectric material.Specific embodiment is as follows：
Embodiment 1
(1) by MgO, TiO2、Al2O3、Nb2O5And Li2CO3Stoichiometrically formula Li2Mg3Ti0.75(Al1/2Nb1/2)0.25O6Into Row dispensing, matches and is：2.7647g Li2CO3、4.5239g MgO、2.2194g TiO2, 0.2360g Al2O3, 0.6092g Nb2O5, about 10g powders are put into polyester ball grinder, and raw material is 1 with the mass ratio of absolute ethyl alcohol and zirconia ball:30:15, it is expert at Ball milling 12 hours on planetary ball mill, rotational speed of ball-mill are 400/ turn point；
(2) raw material after step (1) ball milling is respectively put into drying box, is dried in 110 DEG C 5 hours, then crosses 40 mesh Sieve；
(3) powder after step (2) being sieved is put into alumina crucible and is built in moderate oven, in 1000 DEG C of pre-burnings, protects Then temperature 4 hours crosses 40 mesh sieve；
(4) the PVA powder that the powder additional mass percent content after step (3) being sieved is 0.7% mixes, and puts Enter in polyester ball grinder, raw material is 1 with the mass ratio of absolute ethyl alcohol and zirconia ball:30:15, the ball milling on planetary ball mill 12 hours, rotating speed was 400 revs/min and is granulated；
(5) raw material after step (4) ball milling is respectively put into drying box, is dried in 110 DEG C 5 hours, then crosses 80 mesh Sieve；
(6) green compact are made with the pressure of 6MPa with powder compressing machine in the powder of step (5), a diameter of 10mm of green compact is thick Degree is 4~5mm；
(7) green compact of step (6) are kept the temperature 6 hours, high q-factor rock salt class Li is made in 1200 DEG C of sintering2Mg3TiO6Base is micro- Wave dielectric material.
(8) microwave dielectric property of resulting product is tested by Network Analyzer, microwave dielectric property is as follows：
εr=13.02
Qf=162,429GHz (@9.880GHz)
τf=-19.17ppm/ DEG C
Embodiment 2~6
Specific embodiment 2~6 is different content Li2Mg3Ti1-x(Al1/2Nb1/2)xO6, calcined temperature, sintering temperature, burning It ties the time and its microwave dielectric property is as shown in table 1, remaining preparation process and technological parameter are identical with embodiment 1.

Claims (4)

1. a kind of high q-factor rock salt class microwave dielectric material, with MgO, TiO2、Al2O3、Nb2O5And Li2CO3For raw material, pass through solid phase Prepared by method, target synthetic expression formula is Li2Mg3Ti1-x(Al1/2Nb1/2)xO6, wherein 0 x≤0.95 ＜.
The high q-factor rock salt class microwave dielectric material, specific implementation step are as follows：
(1) by MgO, TiO2、Al2O3、Nb2O5And Li2CO3Stoichiometrically formula Li2Mg3Ti1-x(Al1/2Nb1/2)xO6, wherein x=0 ~0.95 carries out dispensing, and powder is put into polyester ball grinder, after absolute ethyl alcohol and zirconia ball is added, ball milling 4~24 hours；
(2) raw material after step (1) ball milling is put into drying box, in 100~120 DEG C of drying, then crosses 40 mesh sieve；
(3) powder after step (2) being sieved is put into alumina crucible and is built in moderate oven, in 900~1100 DEG C of pre-burnings, protects Then temperature 2~8 hours crosses 40 mesh sieve；
(4) the PVA powder that the powder additional mass percent content after step (3) being sieved is 0.7% mixes, and is put into poly- In ester ball grinder, after absolute ethyl alcohol and zirconia ball is added, ball milling is granulated for 4~24 hours；
(5) powder after being granulated step (4) is put into drying box, is dried in 100~120 DEG C 4~6 hours, is then crossed 80 Mesh sieves；
(6) green compact are made with the pressure of 4~8MPa with powder compressing machine in the powder of step (5)；
(7) green compact of step (6) are kept the temperature 2~8 hours, high q-factor rock salt class is made in 1180 DEG C of -1340 DEG C of sintering Li2Mg3TiO6Base microwave dielectric material.
2. a kind of high q-factor rock salt class microwave dielectric material according to claim 1, which is characterized in that the step (1), (4) it is all made of planetary ball mill and carries out ball milling, drum's speed of rotation is 400 revs/min.
3. a kind of high q-factor rock salt class microwave dielectric material according to claim 1, which is characterized in that the step (1), (4) raw material is 1 with the mass ratio of absolute ethyl alcohol and zirconia ball:30:15.
4. a kind of high q-factor rock salt class microwave dielectric material according to claim 1, which is characterized in that the step (6) The a diameter of 10mm of green compact, thickness are 4~5mm.
CN201810200792.5A 2018-03-12 2018-03-12 A kind of high q-factor rock salt class microwave dielectric material Pending CN108314444A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109111225A (en) * 2018-08-16 2019-01-01 天津大学 Regulate and control the lithium titanate base microwave dielectric material of microwave dielectric property by magnesium niobium component
CN110218086A (en) * 2019-05-08 2019-09-10 天津大学 A kind of lithium-based ceramic material of microwave-medium substrate low dielectric constant and high Q value
CN111302794A (en) * 2020-02-07 2020-06-19 天津大学 High-performance rock salt structure medium material and preparation method thereof
CN112457010A (en) * 2020-12-02 2021-03-09 电子科技大学 Rock salt type reconstructed superlattice structure microwave dielectric ceramic material and preparation method thereof
CN114656255A (en) * 2022-03-22 2022-06-24 无锡市高宇晟新材料科技有限公司 Magnesium titanate lithium composite microwave dielectric ceramic material and preparation method thereof

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CN107311646A (en) * 2017-06-19 2017-11-03 天津大学 A kind of preparation method for improving strontium titanate ceramicses dielectric material performance

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CN104692795A (en) * 2015-02-09 2015-06-10 陕西师范大学 Ultra-low-loss lithium magnesium titanate microwave dielectric ceramic material and preparation method thereof
CN106810209A (en) * 2017-01-12 2017-06-09 天津大学 A kind of high q-factor lithium magnesium titanium series microwave dielectric ceramic
CN107311646A (en) * 2017-06-19 2017-11-03 天津大学 A kind of preparation method for improving strontium titanate ceramicses dielectric material performance

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109111225A (en) * 2018-08-16 2019-01-01 天津大学 Regulate and control the lithium titanate base microwave dielectric material of microwave dielectric property by magnesium niobium component
CN110218086A (en) * 2019-05-08 2019-09-10 天津大学 A kind of lithium-based ceramic material of microwave-medium substrate low dielectric constant and high Q value
CN111302794A (en) * 2020-02-07 2020-06-19 天津大学 High-performance rock salt structure medium material and preparation method thereof
CN112457010A (en) * 2020-12-02 2021-03-09 电子科技大学 Rock salt type reconstructed superlattice structure microwave dielectric ceramic material and preparation method thereof
CN114656255A (en) * 2022-03-22 2022-06-24 无锡市高宇晟新材料科技有限公司 Magnesium titanate lithium composite microwave dielectric ceramic material and preparation method thereof
CN114656255B (en) * 2022-03-22 2023-06-30 无锡市高宇晟新材料科技有限公司 Magnesium lithium titanate composite microwave dielectric ceramic material and preparation method thereof

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Application publication date: 20180724