CN101092300A - Dielectric adjustable material of ceramics burned together at low temperature, and preparation method - Google Patents

Dielectric adjustable material of ceramics burned together at low temperature, and preparation method Download PDF

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CN101092300A
CN101092300A CN 200610027784 CN200610027784A CN101092300A CN 101092300 A CN101092300 A CN 101092300A CN 200610027784 CN200610027784 CN 200610027784 CN 200610027784 A CN200610027784 A CN 200610027784A CN 101092300 A CN101092300 A CN 101092300A
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low
mgo
tio
sintering
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CN100457678C (en
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翟继卫
丑修建
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Tongji University
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Tongji University
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Abstract

This invention relates to a method for preparing ceramic material with a sintering temperature below 950 deg.C. The ceramic material is composed of Ba1-xSrxTiO3 (x = 0.2 -0.6) 75.0-95.0 wt. %, MgO 0.15-15 wt. %, B2O3 0-1.0 wt. %, Li2CO3 3.0-10.0 wt. %. The method utilizes MgO and B2O3-Li2O sintering aid to dope and modify BST ceramic material, and the obtained ceramic material has such advantages as adjustable dielectric constant (100-2000) and low sintering temperature (850-950 deg.C). The ceramic material can be used in LTCC technique and microwave adjustable devices.

Description

Low-temperature co-burning ceramic material that a kind of dielectric is adjustable and preparation method thereof
Technical field
The invention belongs to electronic material and device technology field, be specifically related to a kind of sintering temperature at stupalith below 950 ℃ and preparation method thereof.
Background technology
Fast development of information technology, an urgent demand high-speed data and high current density transmission, electronic circuit develops to direction microminiaturized, integrated and high frequencyization day by day, this just to electronic component proposed that size is small, the requirement of high frequency, high reliability, with low cost and high integration.LTCC (LTCC) technology is integrated into element and circuit on the multilayer ceramic substrate with mode of printing exactly, again by low-temperature primary sintering, element is stably imbedded in the board structure, thereby reaches the purpose of the integrated and product miniaturization of element heights.
For the LTCC technology,, not only can solve the package dimension limit problem of slice component, and have the following advantages as the integrated mainstream technology of passive element:
(1) in 2.4MHz～80GHz range of frequency, the loss of signal that the LTCC technology is brought is well below the multilayer line plate technique;
(2) owing to the introducing of batch process equipment and technology, material cost reduces and carries out processing and manufacturing in China, and the cost of LTCC product is significantly reduced;
(3) owing to use the element pasted on surface that embeds on element rather than the wiring board, module size reduces 20%～40%, and system cost is lower;
(4) satisfy in the electronic module material of wireless application RF range of frequency requirement, the LTCC material is optimal material.
The LTCC technology is exploitation of LTCC device and an importance of producing with the high-performance electronic material, utilizing the electricity of ferroelectric ceramic material non-linear is the important technology approach that realizes the passive tunable microwave device, and Application and Development has become current research focus in the BST of microwave adjustable device low-temperature co-burning ceramic material.
In recent years, strontium-barium titanate (BST) stupalith has great significance in microwave adjustable device (phase shifter, wave filter etc.) Application Areas owing under the DC electric field effect, have the adjustable excellent dielectric properties of nonlinear dielectric constant.But, adopting traditional electronic ceramic technology, the sintering temperature of BST pottery is generally more than 1350 ℃, and so high sintering temperature can not be burnt altogether with cheap silver, copper electrode material substantially, is difficult to satisfy the technical requirements of LTCC.In addition,, generally have high specific inductivity,, require material to have proper dielectric constant, could satisfy impedance matching in the microwave adjustable device application facet for the BST stupalith.Therefore, the LTCC technology is just guaranteeing that material possesses under the prerequisite of suitable dielectric properties (specific inductivity, low-and high-frequency dielectric loss and adjustability etc.) with the crucial difficult point of BST stupalith exploitation, how to solve low-temperature sintering (promptly burning altogether with cheap silver, the copper electrode material) problem of material.
Means for the dielectric properties that improve the BST material are mainly still passed through doping vario-property, United States Patent (USP) us5,635,434 " Louise Sengupta, Warwick.Ceramic Ferroelectric Composite Material-BSTO-MagnesiumBased ompound. " report utilizes Mg class properties-correcting agent (MgO, MgZrO 3, MgAl 2O 4, MgTiO 3) coming modification, Mg class properties-correcting agent all has significant effect to the specific inductivity that reduces the BST pottery, and MgO is best to the low frequency loss effect that reduces the BST pottery, but the voltage adjustability of material is descended; Though these doping by Mg class properties-correcting agent effectively reduce the specific inductivity and the dielectric loss of BST pottery, sintering temperature can not satisfy the requirement of LTCC technology substantially all more than 1350 ℃.
Method about the sintering temperature that reduces the BST stupalith mainly contains: (1) adds low melting point oxide or glassy phase sintering aid, as B 2O 3, Li 2O, Zn/Ba-B-Si glass etc.; (2) select advanced preparation technology and means for use, as sol-gel method, hydrothermal method etc.; (3) use hyperfine particulate starting material, as nano-powder, superfine powder raw material etc.The research work that reduces the BST ceramic sintering temperature by doping low melting point oxide or glassy phase sintering aid has many reports, as document " S.M.Rhim, S.Hong, H.Bak, et al..Effects of B 2O 3Addition on the Dielectric andFerroelectric Properties of Ba 0.7Sr 0.3TiO 3Ceramics.J.Am.Ceram.Soc., 2000,83 (5): 1145-1148 " by adding 0.5wt%B 2O 3, the sintering temperature of BST pottery is reduced to 1150 ℃, its dielectric properties remain unchanged substantially.Document " Matjaz Valant, Danilo Suvorov.Low-Temperature Sintering of (Ba 0.6Sr 0.4) TiO 3.J.Am.Ceram.Soc., 2004,87 (7): the 1222-1226 " Li of employing 0.4wt% 2During the O doped BST, sintering temperature can be reduced to 900 ℃, and its dielectric loss and adjustability are respectively 0.0045 and 13.5% (test frequency is 1MHz, and applying direct current electric field is 30kV/cm), has a small amount of dephasign to produce simultaneously.Document " T.Hu, H.Jantunen, A.Uusimaki, et al..Ba 0.7Sr 0.3TiO 3Powders with B 2O 3Additive Prepared by the Sol-Gel Methodfor Use as Microwave Material.Mater.Sci.Semiconduct.Process., 2002,5 (2-3): 215-221 " Ba that obtains by sol-gel method 0.7Sr 0.3TiO 3Superfine powder, same by adding B 2O 3And Li 2The O sintering agent, Ba 0.7Sr 0.3TiO 3Ceramic sintering temperature also can drop to 900C, and at ambient temperature, the specific inductivity that obtains under the 1kHz test frequency is 4290, and loss reaches 0.005, and adjustability is not seen its report, and it is higher relatively to adopt sol-gel technology to obtain BST powder cost.Document " Cheng Huarong, Zhu Jingchuan, Quan Zaihao etc. sintering process is to B 2O 3Doping Ba 1-xSr xTiO 3The influence of graded ceramics dielectric properties. Journal of Inorganic Materials, 2005,20 (5): 1145-1152 " be reported among the BST suitably doping B 2O 3Reduced by 150 ℃ than the identical component BST ceramic sintering temperature that do not mix, but dielectric properties are relatively poor, B 2O 3Doping 0.5wt%, loss reaches 0.095 under the room temperature.These single interpolations by B203 and Li02 sintering agent have reduced the sintering temperature of BST pottery, but that specific inductivity still keeps is higher, more than 2000, therefore also are difficult to the space impedance matching requirement of composite microwave device.
At present, specific inductivity is suitable, and the energy low-temperature sintering, and the BST stupalith that is suitable for the application of LTCC technology and microwave adjustable device yet there are no report.
Summary of the invention
One of purpose of the present invention provides a kind of low-temperature sintered ceramics material with dielectric adjustable.
Another object of the present invention provides above-mentioned this low-temperature sintered ceramics preparation methods with dielectric adjustable.
Design of the present invention is such: because Mg class properties-correcting agent all has significant effect to the specific inductivity that reduces the BST pottery, add low melting point oxide or glassy phase sintering aid and can reduce sintering temperature, so attempt adopting simultaneously the method for magnesium class properties-correcting agent and sintering agent, choose the sort of properties-correcting agent of concrete application and sintering agent by test, and the effective content of definite each component, thereby obtaining specific inductivity can change in seriation, and the low sintering BST stupalith of energy is suitable for the application of LTCC technology and microwave adjustable device.
For reaching above-mentioned purpose, the technical solution used in the present invention is as follows:
A kind of low-temperature sintered ceramics material, each component and mass percent thereof are:
Ba (1-x)Sr xTiO 3(x＝0.2～0.6) 75.0wt％～95.0wt％
MgO 0.15wt％～15wt％
B 2O 3 0wt％～1.0wt％
Li 2CO 3 3.0wt％～10.0wt％。
Above-mentioned low-temperature sintered ceramics material, the preferred scheme of each component and mass percent thereof is:
Ba (1-x)Sr xTiO 3(x＝0.2～0.6) 80.0wt％～95.0wt％
MgO 0.15wt％～5wt％
B 2O 3 0wt％～0.75wt％
Li 2CO 3 4.0wt％～10.0wt％。
Low-temperature sintered ceramics material preparation method provided by the present invention comprises the steps:
Take by weighing Ba by proportioning (1-x)Sr xTiO 3(x=0.2～0.6) powder, MgO, B 2O 3And Li 2CO 3, add zirconia ball and dehydrated alcohol or water, ball milling 20～24 hours, the discharging oven dry grinds to form powder, crosses 200 mesh sieves and promptly gets described low-temperature co-burning ceramic material.
The stupalith powder of above-mentioned preparation can be made into ceramics sample or device by prior art, or ceramic thick film etc.If temporarily need not, the powder that obtains can be pulverized after 2～3 hours 300 ℃～500 ℃ calcinings, behind 200 mesh sieves, preserve.
Described Ba (1-x)Sr xTiO 3(x=0.2～0.6) powder is to make according to traditional electronic ceramic powder preparation technology, by solid reaction process, selects BaTiO for use 3And SrTiO 3(99.9%, 100nm, Shandong state rises ceramic material company limited and provides) be main raw material, according to certain Ba/Sr molar ratio ingredient, confected materials is placed nylon ball grinder, added zirconia ball and dehydrated alcohol or deionized water ball milling 24 hours, discharging oven dry back obtains Ba 1100 ℃ of pre-burnings 4 hours after the grinding (1-x)Sr xTiO 3(x=0.2～0.6) powder.
The proportioning of each feed composition is with the mass percent of each component in the finished-product material during preparation.
During ball milling, zirconia ball and ceramic powder (are Ba (1-x)Sr xTiO 3(x=0.2～0.6) powder, MgO, B 2O 3And Li 2CO 3Compound) mass ratio be preferably 1.0～2.0: 1; The mass ratio of dehydrated alcohol or water and ball-milling ceramic powder is preferably 0.5～1.5: 1.
The low-temperature co-burning ceramic material that this method obtains, if adopt traditional electronic ceramic technology, by after wherein adding an amount of binding agent granulation, can make ceramics sample or device through dry-pressing or cold isostatic compaction, the sticking back of row sintering under 850 ℃～950 ℃ air atmosphere, insulation can be used more than 4 hours; In addition, also described low-temperature co-burning ceramic material can be made ceramic size, make ceramic thick film by flow casting molding or thick film screen printing technology, after 300 ℃～500 ℃ dry heat are handled, can obtain the ceramic green band of different thickness, can burn altogether with copper, silver electrode material at 800 ℃～950 ℃, be applicable to LTCC technology and multilayer circuit plate technique.
The present invention adopts B 2O 3And Li 2CO 3As sintering aid, play the effect of liquid phase sintering, reduce the sintering temperature of BST pottery; Simultaneously, select for use MgO as the doping vario-property agent, by the doping of adjustment MgO doping agent, thus the dielectric properties of change and control BST stupalith, it has following principal feature:
(1) sintering temperature is low, can adjust B according to the different components proportioning 2O 3And Li 2CO 3The addition of sintering aid, sintering temperature can be reduced between 800 ℃～950 ℃, and sintering atmosphere is an oxygen atmosphere.
(2) variation of the doping by MgO and the adjustment of Ba/Sr ratio, specific inductivity is adjustable continuously between 100～2000, and dielectric loss can be controlled at below 0.005.
(3) under the applying direct current electric field effect, described stupalith has dielectric, nonlinear, and specific inductivity is adjustable with extra electric field.With the doping difference of MgO, its adjustability can change between 10%～50% (40kV/cm).
(4) preparation technology is simple, and cost is low, and the side effect of material system environment-protecting asepsis is applicable to multilayer circuit plate technique and low temperature co-fired technology.The present invention is by MgO properties-correcting agent and B 2O 3-Li 2In the time of the O sintering agent BST stupalith is carried out composite doping modification, thereby obtained specific inductivity and can seriation change (100～2000), and the BST stupalith of energy low-temperature sintering (850 ℃～950 ℃) is suitable for the application of LTCC technology and microwave adjustable device.
Description of drawings
Fig. 1 is the different proportioning Ba 900 ℃ of sintering preparations 0.6Sr 0.4TiO 3The relation curve of the specific inductivity of-MgO ceramics sample and loss and temperature.
Fig. 2 is the different proportioning Ba 900 ℃ of sintering preparations 0.6Sr 0.4TiO 3The relation curve of the specific inductivity of-MgO ceramics sample and external dc field intensity.
Embodiment
Embodiment 1～3
Preparation Ba 0.6Sr 0.4TiO 3-MgO LTCC:
Select BaTiO for use 3And SrTiO 3(99.9%, 100nm, Shandong state rises ceramic material company limited and provides) be main raw material, according to Ba: Sr=6: 4 (mol ratios) batching, confected materials is placed nylon ball grinder, added zirconia ball and dehydrated alcohol ball milling 24 hours, discharging oven dry back obtains Ba 1100 ℃ of pre-burnings 4 hours after the grinding 0.6Sr 0.4TiO 3Powder is stand-by.
Take by weighing chemical reagent by following different components proportioning:
Experimental formula Ba 0.6Sr 0.4TiO 3 MgO B 2O 3 Li 2CO 3
Embodiment 1 13.9775g 0.0225g - 1.0g
Embodiment 2 13.525g 0.375g 0.1g 1.0g
Embodiment 3 13.150g 0.75g 0.1g 1.0g
The above-mentioned compound of respectively filling a prescription is put into nylon ball grinder respectively, added 20g zirconia ball and 30g dehydrated alcohol ball milling 24 hours, discharging oven dry back powder is crossed 200 mesh sieves, and according to traditional electronic ceramic technology, the polyvinyl alcohol (PVA) of employing 8% carries out granulation as binding agent, under 10MPa pressure, dry method is pressed into diameter phi=10mm green sheet, under air atmosphere, through 900 ℃ of sintering, be incubated after 5 hours, obtain different ingredients B respectively 2O 3-Li 2The adulterated Ba of O 0.6Sr 0.4TiO 3/ MgO composite ceramics sample.With the ceramics sample polishing both surfaces that makes, carried out the dielectric properties test behind silver, the silver ink firing.Embodiment 1～3 prepared ceramics sample dielectric properties are seen accompanying drawing 1 and Fig. 2, and a, b, c are respectively the ceramics sample of embodiment 1,2 and 3 among the figure.

Claims (6)

1, a kind of low-temperature sintered ceramics material, each component and mass percent thereof are:
Ba (1-x)Sr xTiO 3(x＝0.2～0.6) 75.0wt％～95.0wt％
MgO 0.15wt％～15wt％
B 2O 3 0wt％～1.0wt％
Li 2CO 3 3.0wt％～10.0wt％。
2, low-temperature sintered ceramics material as claimed in claim 1, each component and mass percent thereof are:
Ba (1-x)Sr xTiO 3(x＝0.2～0.6) 80.0wt％～95.0wt％
MgO 0.15wt％～5wt％
B 2O 3 0wt％～0.75wt％
Li 2CO 3 4.0wt％～10.0wt％。
3, the preparation point-score of claim 1 or 2 described low-temperature sintered ceramics materials the steps include: to take by weighing Ba by each set of dispense ratio (1-x)Sr xTiO 3(x=0.2～0.6), MgO, B 2O 3And Li 2CO 3, add zirconia ball and dehydrated alcohol or deionized water, ball milling 20～24 hours, the discharging oven dry grinds to form powder then, crosses 200 mesh sieves at last and gets final product.
4, the preparation point-score of low-temperature sintered ceramics material as claimed in claim 3 is characterized in that: the powder that oven dry obtains is pulverized after 2～3 hours 300 ℃～500 ℃ calcinings, after 200 mesh sieves.
5, the preparation point-score of low-temperature sintered ceramics material as claimed in claim 3 is characterized in that: the mass ratio of zirconia ball and ceramic powder is 1.0～2.0: 1.
6, the preparation point-score of low-temperature sintered ceramics material as claimed in claim 3 is characterized in that: the mass ratio of dehydrated alcohol or deionized water and ball-milling ceramic powder is 0.5～1.5: 1.
CNB2006100277842A 2006-06-19 2006-06-19 Dielectric adjustable material of ceramics burned together at low temperature, and preparation method Expired - Fee Related CN100457678C (en)

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Cited By (10)

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WO2011029286A1 (en) * 2009-09-10 2011-03-17 中国矿业大学(北京) Composite sintering agent and method for preparing nano crystalline ceramics at low temperature using the same
CN102408232A (en) * 2011-08-22 2012-04-11 天津大学 Method for preparing BST-MgO (barium strontium titanate-magnesium oxide) based ceramic tape-casting slurry and blanks
CN102503412A (en) * 2011-11-11 2012-06-20 天津大学 Barium strontium titanate-based ferroelectric ceramic material with controllable dielectric constant and temperature characteristic and preparation method thereof
CN102633500A (en) * 2012-04-18 2012-08-15 同济大学 Dielectric-adjustable low-temperature co-firing ceramic material and preparation method thereof
CN102848285A (en) * 2012-09-11 2013-01-02 中国兵器工业集团第二一四研究所苏州研发中心 Chamfering method of LTCC chip component and grinding material formula
CN102863223A (en) * 2012-09-11 2013-01-09 中国兵器工业集团第二一四研究所苏州研发中心 Large-size low temperature cofired ceramic (LTCC) substrate sintering process
CN102863221A (en) * 2012-09-20 2013-01-09 广东风华高新科技股份有限公司 Method, sintering aid and materials for preparation of low-temperature cofired medium ceramic and application
CN105860596A (en) * 2014-12-05 2016-08-17 三祥新材股份有限公司 Method for improving specific surface area and reaction activity of fused zirconia
CN108470824A (en) * 2018-03-15 2018-08-31 南方科技大学 High-temperature-resistant multilayer piezoelectric ceramic actuator and preparation method and application thereof
CN114163229A (en) * 2021-12-31 2022-03-11 无锡市高宇晟新材料科技有限公司 Microwave dielectric ceramic material and preparation method thereof

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Cited By (14)

* Cited by examiner, † Cited by third party
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WO2011029286A1 (en) * 2009-09-10 2011-03-17 中国矿业大学(北京) Composite sintering agent and method for preparing nano crystalline ceramics at low temperature using the same
CN102408232A (en) * 2011-08-22 2012-04-11 天津大学 Method for preparing BST-MgO (barium strontium titanate-magnesium oxide) based ceramic tape-casting slurry and blanks
CN102503412A (en) * 2011-11-11 2012-06-20 天津大学 Barium strontium titanate-based ferroelectric ceramic material with controllable dielectric constant and temperature characteristic and preparation method thereof
CN102633500B (en) * 2012-04-18 2014-04-02 同济大学 Dielectric-adjustable low-temperature co-firing ceramic material and preparation method thereof
CN102633500A (en) * 2012-04-18 2012-08-15 同济大学 Dielectric-adjustable low-temperature co-firing ceramic material and preparation method thereof
CN102848285B (en) * 2012-09-11 2016-04-13 中国兵器工业集团第二一四研究所苏州研发中心 A kind of LTCC slice component chamfering method and abrasive material formula
CN102863223A (en) * 2012-09-11 2013-01-09 中国兵器工业集团第二一四研究所苏州研发中心 Large-size low temperature cofired ceramic (LTCC) substrate sintering process
CN102863223B (en) * 2012-09-11 2015-02-25 中国兵器工业集团第二一四研究所苏州研发中心 Large-size low temperature cofired ceramic (LTCC) substrate sintering process
CN102848285A (en) * 2012-09-11 2013-01-02 中国兵器工业集团第二一四研究所苏州研发中心 Chamfering method of LTCC chip component and grinding material formula
CN102863221A (en) * 2012-09-20 2013-01-09 广东风华高新科技股份有限公司 Method, sintering aid and materials for preparation of low-temperature cofired medium ceramic and application
CN105860596A (en) * 2014-12-05 2016-08-17 三祥新材股份有限公司 Method for improving specific surface area and reaction activity of fused zirconia
CN105860596B (en) * 2014-12-05 2017-11-24 三祥新材股份有限公司 A kind of method for improving electric-melting zirconia specific surface area and reactivity
CN108470824A (en) * 2018-03-15 2018-08-31 南方科技大学 High-temperature-resistant multilayer piezoelectric ceramic actuator and preparation method and application thereof
CN114163229A (en) * 2021-12-31 2022-03-11 无锡市高宇晟新材料科技有限公司 Microwave dielectric ceramic material and preparation method thereof

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