CN103896579A - Lithium-based low-temperature sintering microwave dielectric ceramic material and preparation method thereof - Google Patents

Lithium-based low-temperature sintering microwave dielectric ceramic material and preparation method thereof Download PDF

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CN103896579A
CN103896579A CN201410105845.7A CN201410105845A CN103896579A CN 103896579 A CN103896579 A CN 103896579A CN 201410105845 A CN201410105845 A CN 201410105845A CN 103896579 A CN103896579 A CN 103896579A
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郑勇
吕学鹏
董作为
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Nanjing University of Aeronautics and Astronautics
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Abstract

本发明公开了一种锂基低温烧结微波介质陶瓷材料及其制备方法，配方的化学组成表达式为：Li2ATi3O8+B2O3，其中A为Zn,Mg,Co,Ni离子中的一种，所述B2O3的添加量相当于Li2ATi3O8的xwt%，其中1.0≤x≤2.50；该陶瓷的制备工艺依次如下：首先将Li2CO3、ZnO、MgO、CoO、NiO和TiO2粉末按配方通式Li2ATi3O8的化学计量比配制基料，其中A为Zn,Mg,Co,Ni离子中的一种，然后直接加入相当于基料重量1%～2.5%的B2O3粉末，经过球磨、压制成型、反应烧结得到产品；产品烧结温度可降至900℃以下，相对介电常数εr在22～26.5内可调，品质因数Qf为21000～63400GHz，谐振频率温度系数τf在-16.0～7.0ppm/℃内可调，可以应用于制造片式多层微波器件，将使该类材料在微波通信方面的应用范围更加广泛。The invention discloses a lithium-based low-temperature sintered microwave dielectric ceramic material and a preparation method thereof. The chemical composition expression of the formula is: Li 2 ATi 3 O 8 +B 2 O 3 , wherein A is Zn, Mg, Co, Ni ions One of the above, the amount of B 2 O 3 added is equivalent to xwt% of Li 2 ATi 3 O 8 , where 1.0≤x≤2.50; the preparation process of the ceramic is as follows: first Li 2 CO 3 , ZnO, MgO, CoO, NiO and TiO 2 powders are formulated as base materials according to the stoichiometric ratio of the general formula Li 2 ATi 3 O 8 , where A is one of Zn, Mg, Co, and Ni ions, and then directly added into the base material The B 2 O 3 powder with a weight of 1% to 2.5% is obtained through ball milling, compression molding, and reaction sintering; the sintering temperature of the product can be lowered to below 900°C, and the relative dielectric constant ε r is adjustable within 22 to 26.5, and the quality factor Qf ranges from 21000 to 63400 GHz, and the resonant frequency temperature coefficient τ f is adjustable within -16.0 to 7.0 ppm/°C. It can be applied to the manufacture of chip multilayer microwave devices, which will make this type of material more widely used in microwave communications.

Description

A kind of low temperature sintering lithium-base microwave dielectric ceramic material and preparation method thereof
Technical field
The invention belongs to electronic ceramics and preparation field thereof, relate in particular to a kind of low temperature sintering lithium-base microwave dielectric ceramic material and preparation method thereof.
Background technology
Microwave-medium ceramics refers to and is applied to microwave frequency band, be mainly in the circuit of UHF, SHF frequency range as dielectric material and complete the stupalith of one or more functions, be the critical material of the microwave devices such as widely used resonator in modern communications field, wave filter, medium substrate, medium guided wave loop.Along with electronic information technology is constantly to high frequency and digitizing future development, miniaturization, integrated and modular requirement to components and parts are day by day urgent, LTCC LTCC(LowTemperature Co-firedCeramics) technology is because of its excellent electricity, machinery, calorifics, operational characteristic and high reliability, become one of major technique of electronic-component module.Compared with other integrated technology, it is low that LTCC technology has sintering temperature, the low metal of available resistivity, as the conductor material of multilayer wiring, can improve packing density, signaling rate, and can in be embedded in the advantages such as the various laminar microwave electronic devices of multilager base plate once-firing.LTCC Technology Need microwave-medium ceramics can burn altogether with electrode in the metal A g of high conductivity low melting point, Cu, and therefore, the low-temperature sintering of microwave dielectric ceramic materials has become study hotspot.Although the microwave-medium ceramics of most of commercial has good microwave dielectric property, its sintering temperature very high (generally higher than 1200 ℃), therefore must research and develop microwave-medium ceramics that intrinsic sintering temperature is lower to meet the requirement of LTCC technique.
Li 2aTi 3o 8the sintering temperature of (A=Zn, Mg, Co, the one in Ni ion) base pottery is conventionally 1100 ℃ of left and right, is the grow a lot lower microwave-medium ceramics system of intrinsic sintering temperature of potentiality of a kind of tool.2010, people's reported first such as S.George Li 2znTi 3o 8and Li 2mgTi 3o 8the sintering characteristic of system and microwave dielectric property.2011, people's reported first such as FangLiang Li 2coTi 3o 8the sintering characteristic of system and microwave dielectric property.The pottery of these systems all has lower sintering temperature and excellent microwave dielectric property, and after calcining, is passing through to add a small amount of sintering aid as B 2o 3, Bi 2o 3, ZnO-B 2o 3glass powder, ZnO-B 2o 3-SiO 2glass powder and ZnO-La 2o 3-B 2o 3glass powder etc., can be reduced to 900 ℃ of left and right by their final sintering temperature, have met the requirement of LTCC Technology.But due to the density that adds membership reduction stupalith of sintering aid, therefore its microwave dielectric property can decline more.
At present when the above-mentioned lithium-based microwave media ceramic of preparation, employing be all traditional solid sintering technology, the method technological process is more complicated, need through calcining+final two stages of sintering, sintering time is longer, and energy consumption is higher, and because process procedure is more, easily bring impurity into, thereby affect the performance of material.Reaction sintering is a kind of simple sintering method, the reaction of raw material powder and densification realize in once sintered process, have saved calcining and secondary ball milling operation in traditional preparation method, can simplify preparation section, reduce production costs and energy consumption, reduce the impurity of bringing in production process.Because powder in reaction sintering does not pass through calcination stage, while therefore adopting reaction sintering to prepare higher ceramic of density, the having relatively high expectations of the purity to material powder and granularity, or need high temperature of reaction.Prepare single-phase Li when adopting reaction sintering 2aTi 3o 8in (A=Zn, Mg, Co, the one in Ni ion) base when pottery,, because temperature of reaction is higher, Li, Zn element are volatile, produce pore, and Li in sintering process 2cO 3raw material decomposes generation CO 2gas can reduce the density of sintered compact, the single-phase Li that therefore adopts reaction sintering directly to prepare 2aTi 3o 8(A=Zn, Mg, Co, the one in Ni ion) base ceramic dense degree is generally lower, causes its microwave dielectric property also to decline accordingly.Along with developing rapidly of modern communications technology, design a kind of microwave dielectric property excellence, low temperature sintering lithium-base microwave dielectric ceramic material that quality stability is good and preparation method thereof, to meet the need of market, is very important.
Summary of the invention
The technical problem solving:
The application is higher for the complex process existing in prior art, energy consumption, microwave dielectric property and the technical problem such as quality stability is poor, and a kind of low temperature sintering lithium-base microwave dielectric ceramic material and preparation method thereof is provided.
Technical scheme:
A kind of low temperature sintering lithium-base microwave dielectric ceramic material, the chemical constitution expression formula of its formula is: Li 2aTi 3o 8+ B 2o 3, wherein A is Zn, Mg, Co, the one in Ni ion, described B 2o 3addition be equivalent to Li 2aTi 3o 8xwt%, wherein 1.0≤x≤2.5.
A preparation method for low temperature sintering lithium-base microwave dielectric ceramic material, step is:
The first step, batching: by Li 2cO 3, AO and TiO 2powder is by formula general formula Li 2aTi 3o 8stoichiometric ratio preparation base-material, wherein A is Zn, Mg, Co, the one in Ni ion, then directly adds the B that is equivalent to base-material weight 1%～2.5% 2o 3powder, obtains compound;
Second step, ball milling: compound is placed in to planetary ball mill wet ball grinding 12～24 hours, and described planetary ball mill rotating speed is 300rpm;
The 3rd step, adds forming agent, granulation: the polyvinyl alcohol water solution that the concentration that adds compound weight 5～8wt% is 5wt%, the granulation of sieving after being dried;
The 4th step, compression moulding: on pressing machine, be pressed into base substrate with the pressure of 100～150MPa;
The 5th step, remove forming agent, sintering: base substrate is risen to 550 ℃ and be incubated 4 hours to remove polyvinyl alcohol forming agent with the temperature rise rate of 1.5 ℃/min in high-temperature box type electric furnace, be warming up to subsequently 800～900 ℃ of sintering 4～8 hours, obtain low temperature sintering lithium-base microwave dielectric ceramic material.
As a preferred technical solution of the present invention: sieving in described the 3rd step is to sieve through 40-60 object screen cloth.
As a preferred technical solution of the present invention: in described the 4th step, base substrate is shaped as right cylinder.
Beneficial effect:
Compared to the prior art a kind of low temperature sintering lithium-base microwave dielectric ceramic material of the present invention and preparation method thereof adopts above technical scheme, there is following technique effect: 1, technological process simple, saved calcining and secondary ball milling operation in traditional preparation method, simplify preparation section, reduce production costs and energy consumption, and reduce the impurity of bringing in production process; 2, cheap, the sintering temperature of raw materials cost is lower than 900 ℃; 3, B in sintering process 2o 3directly mix B with raw material powder 2o 3in reaction sintering process subsequently with raw material in Li 2cO 3form eutectic compound with the powdered reaction such as ZnO, form at a lower temperature liquid phase, not only shorten the distance of material diffusion, promote the synthetic of principal crystalline phase, and residual pore after can blanketing gas overflowing, the carrying out that promotes densification process, finally can obtain the ceramic product of high-compactness by low temperature reaction sintering, and in product, there is no the generation of second-phase; 4, product microwave dielectric property excellence, relative permittivity ε r22～26.5 interior adjustable, quality factor q f is 21000～63400GHz, temperature coefficient of resonance frequency τ fadjustable in-16.0～7.0ppm/ ℃; 5, product microwave dielectric property and quality stability are good, can be applied to and manufacture chip multilayer microwave device, thereby the not division of history into periods of widespread production is for current material.
Embodiment:
Further illustrate technique effect of the present invention below in conjunction with example.
Table 1 is the compound of 12 kinds of component prescriptions.
The composition proportion of 12 kinds of compounds of table 1
Figure BDA0000479821500000031
Embodiment 1:
The first step: by Li 2cO 3, AO and TiO 2powder is by formula general formula Li 2aTi 3o 8stoichiometric ratio preparation base-material, wherein A is Zn, Mg, Co, the one in Ni ion, then requires to add B according to composition described in table 1 2o 3powder, obtains compound;
Second step: compound is placed in to planetary ball mill wet ball grinding 12 hours, and described planetary ball mill rotating speed is 300rpm;
The 3rd step: the polyvinyl alcohol water solution that the concentration that adds compound weight 5wt% is 5wt%, the dry rear 40-60 eye mesh screen granulation of crossing;
The 4th step: on pressing machine, be pressed into right cylinder base substrate with the pressure of 100MPa;
The 5th step: base substrate is risen to 550 ℃ and be incubated 4 hours to remove polyvinyl alcohol forming agent with the temperature rise rate of 1.5 ℃/min in high-temperature box type electric furnace, be warming up to subsequently 800 ℃ of sintering 8 hours, obtain low temperature sintering lithium-base microwave dielectric ceramic material.
Under above-mentioned preparation process condition, be prepared into lithium-based microwave media ceramic, and measured respectively its DIELECTRIC CONSTANT ε r, quality factor q f value and temperature coefficient of resonance frequency τ f, the microwave dielectric property of the lithium-based microwave media ceramic of heterogeneity proportioning is in table 2.
Table 2 adopts embodiment 1 to prepare the microwave dielectric property of different lithium base microwave dielectric ceramics
Figure BDA0000479821500000041
Embodiment 2:
The first step: by Li 2cO 3, AO and TiO 2powder is by formula general formula Li 2aTi 3o 8stoichiometric ratio preparation base-material, wherein A is Zn, Mg, Co, the one in Ni ion, then requires to add B according to composition described in table 1 2o 3powder, obtains compound;
Second step: compound is placed in to planetary ball mill wet ball grinding 24 hours, and described planetary ball mill rotating speed is 300rpm;
The 3rd step: the polyvinyl alcohol water solution that the concentration that adds compound weight 8wt% is 5wt%, the dry rear 40-60 eye mesh screen granulation of crossing;
The 4th step: on pressing machine, be pressed into right cylinder base substrate with the pressure of 150MPa;
The 5th step: base substrate is risen to 550 ℃ and be incubated 4 hours to remove polyvinyl alcohol forming agent with the temperature rise rate of 1.5 ℃/min in high-temperature box type electric furnace, be warming up to subsequently 900 ℃ of sintering 4 hours, obtain low temperature sintering lithium-base microwave dielectric ceramic material.
Under above-mentioned preparation process condition, be prepared into lithium-based microwave media ceramic, and measured respectively its DIELECTRIC CONSTANT ε r, quality factor q f value and temperature coefficient of resonance frequency τ f, the microwave dielectric property of the lithium-based microwave media ceramic of heterogeneity proportioning is in table 3.
Table 3 adopts embodiment 2 to prepare the microwave dielectric property of different lithium base microwave dielectric ceramics
Figure BDA0000479821500000042
Embodiment 3:
The first step: by Li 2cO 3, AO and TiO 2powder is by formula general formula Li 2aTi 3o 8stoichiometric ratio preparation base-material, wherein A is Zn, Mg, Co, the one in Ni ion, then requires to add B according to composition described in table 1 2o 3powder, obtains compound;
Second step: compound is placed in to planetary ball mill wet ball grinding 20 hours, and described planetary ball mill rotating speed is 300rpm;
The 3rd step: the polyvinyl alcohol water solution that the concentration that adds compound weight 6wt% is 5wt%, the dry rear 40-60 eye mesh screen granulation of crossing;
The 4th step: on pressing machine, be pressed into right cylinder base substrate with the pressure of 120MPa;
The 5th step: base substrate is risen to 550 ℃ and be incubated 4 hours to remove polyvinyl alcohol forming agent with the temperature rise rate of 1.5 ℃/min in high-temperature box type electric furnace, be warming up to subsequently 850 ℃ of sintering 6 hours, obtain low temperature sintering lithium-base microwave dielectric ceramic material.
Under above-mentioned preparation process condition, be prepared into lithium-based microwave media ceramic, and measured respectively its DIELECTRIC CONSTANT ε r, quality factor q f value and temperature coefficient of resonance frequency τ f, the microwave dielectric property of the lithium-based microwave media ceramic of heterogeneity proportioning is in table 4.
Table 4 adopts embodiment 3 to prepare the microwave dielectric property of different lithium base microwave dielectric ceramics
Figure BDA0000479821500000051
By the contrast of between table 1, table 2, table 3 and table 4, can draw:
1,, in the time that in lithium-based microwave media ceramic, A is Zn, the dielectric loss of gained lithium-based microwave media ceramic is relatively low.
2, in the time that in lithium-based microwave media ceramic, A is Co and Ni, the temperature coefficient of resonance frequency relatively nearly zero of gained lithium-based microwave media ceramic.
3, sintering temperature is relatively large on the impact of microwave dielectric property, and in the time of the sintering temperature value of mediating, when being 850 ℃, the ceramic dielectric loss of above-mentioned formula is relatively low.
Above-described embodiment is just for content of the present invention is set forth, rather than restriction, and therefore any change in implication and the scope suitable with claims of the present invention, all should think to be included in the scope of claims.

Claims (4)

1. a low temperature sintering lithium-base microwave dielectric ceramic material, is characterized in that: the chemical constitution expression formula of described low temperature sintering lithium-base microwave dielectric ceramic material formula is: Li 2aTi 3o 8+ B 2o 3, wherein A is Zn, Mg, Co, the one in Ni ion, described B 2o 3addition be equivalent to Li 2aTi 3o 8x wt%, wherein 1.0≤x≤2.5.
2. a method of preparing low temperature sintering lithium-base microwave dielectric ceramic material described in claim 1, is characterized in that comprising the steps:
The first step, batching: by Li 2cO 3, AO and TiO 2powder is by formula general formula Li 2aTi 3o 8stoichiometric ratio preparation base-material, wherein A is Zn, Mg, Co, the one in Ni ion, then directly adds the B that is equivalent to base-material weight 1%～2.5% 2o 3powder, obtains compound;
Second step, ball milling: compound is placed in to planetary ball mill wet ball grinding 12～24 hours, and described planetary ball mill rotating speed is 300rpm;
The 3rd step, adds forming agent, granulation: the polyvinyl alcohol water solution that the concentration that adds compound weight 5～8wt% is 5wt%, the granulation of sieving after being dried;
The 4th step, compression moulding: on pressing machine, be pressed into base substrate with the pressure of 100～150MPa;
The 5th step, remove forming agent, sintering: base substrate is risen to 550 ℃ and be incubated 4 hours to remove polyvinyl alcohol forming agent with the temperature rise rate of 1.5 ℃/min in high-temperature box type electric furnace, be warming up to subsequently 800～900 ℃ of sintering 4～8 hours, obtain low temperature sintering lithium-base microwave dielectric ceramic material.
3. a kind of method of preparing low temperature sintering lithium-base microwave dielectric ceramic material according to claim 2, is characterized in that: sieving in described the 3rd step is to sieve through 40-60 object screen cloth.
4. a kind of method of preparing low temperature sintering lithium-base microwave dielectric ceramic material according to claim 2, is characterized in that:
In described the 4th step, base substrate is shaped as right cylinder.
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CN104496422A (en) * 2014-12-02 2015-04-08 桂林理工大学 Temperature stable microwave dielectric ceramic Li3Mg2BO5 sintered at low temperature and its preparation method
CN105060878A (en) * 2015-09-11 2015-11-18 天津大学 Microwave dielectric ceramic with low dielectric constant and high quality factor and preparation method thereof
CN106032318A (en) * 2015-03-12 2016-10-19 中国科学院上海硅酸盐研究所 A kind of low temperature co-fired ceramic material and preparation method thereof
CN106116574A (en) * 2016-06-13 2016-11-16 天津大学 A kind of preparation method of low temperature sintering lithium magnesium niobium series microwave dielectric ceramic
CN106145931A (en) * 2016-06-20 2016-11-23 电子科技大学 A kind of Novel super-low loss microwave dielectric ceramic materials and preparation method thereof
CN112608144A (en) * 2020-12-17 2021-04-06 洛阳中超新材料股份有限公司 Lithium-based microwave dielectric ceramic material, preparation method thereof and lithium-based microwave dielectric ceramic
CN113666731A (en) * 2021-08-24 2021-11-19 中国电子科技集团公司第五十八研究所 Silicate microwave dielectric ceramic material and preparation method thereof

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CN103601485A (en) * 2013-11-11 2014-02-26 成都工业学院 Lithium-zinc titanate microwave medium ceramic material prepared by semi-chemical method and preparation method thereof

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CN103601485A (en) * 2013-11-11 2014-02-26 成都工业学院 Lithium-zinc titanate microwave medium ceramic material prepared by semi-chemical method and preparation method thereof

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CN104496422A (en) * 2014-12-02 2015-04-08 桂林理工大学 Temperature stable microwave dielectric ceramic Li3Mg2BO5 sintered at low temperature and its preparation method
CN106032318A (en) * 2015-03-12 2016-10-19 中国科学院上海硅酸盐研究所 A kind of low temperature co-fired ceramic material and preparation method thereof
CN106032318B (en) * 2015-03-12 2018-06-22 中国科学院上海硅酸盐研究所 A kind of low-temperature co-burning ceramic material and preparation method thereof
CN105060878A (en) * 2015-09-11 2015-11-18 天津大学 Microwave dielectric ceramic with low dielectric constant and high quality factor and preparation method thereof
CN106116574A (en) * 2016-06-13 2016-11-16 天津大学 A kind of preparation method of low temperature sintering lithium magnesium niobium series microwave dielectric ceramic
CN106145931A (en) * 2016-06-20 2016-11-23 电子科技大学 A kind of Novel super-low loss microwave dielectric ceramic materials and preparation method thereof
CN106145931B (en) * 2016-06-20 2018-10-26 电子科技大学 A kind of ultra-low loss microwave dielectric ceramic materials and preparation method thereof
CN112608144A (en) * 2020-12-17 2021-04-06 洛阳中超新材料股份有限公司 Lithium-based microwave dielectric ceramic material, preparation method thereof and lithium-based microwave dielectric ceramic
CN112608144B (en) * 2020-12-17 2022-01-28 洛阳中超新材料股份有限公司 Lithium-based microwave dielectric ceramic material, preparation method thereof and lithium-based microwave dielectric ceramic
CN113666731A (en) * 2021-08-24 2021-11-19 中国电子科技集团公司第五十八研究所 Silicate microwave dielectric ceramic material and preparation method thereof

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