CN103183510A - Niobium-magnesium-acid-bismuth based lithium-titanium co-replaced microwave dielectric ceramic material and preparation method thereof - Google Patents
Niobium-magnesium-acid-bismuth based lithium-titanium co-replaced microwave dielectric ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of microwave dielectric ceramic material manufacturing and particularly relates to a niobium-magnesium-acid-bismuth based microwave dielectric ceramic material and a preparation method thereof. The ceramic material comprises the following components in mole percentage by adjusting the reasonable proportions of dielectric function additives: 59%-60% of Bi2O3, 6.9%-7.0% of MgO, 30%-33.2% of Nb2O5, 0.15%-3.0% of Li3CO3 and 0.15%-3.0% of TiO2, wherein the Bi2O3, the MgO and the Nb2O5 are host materials, and the Li3CO3 and the TiO2 are the dielectric function additives. The dielectric constant of niobium-magnesium-acid-bismuth based ceramic material prepared by a conventional solid-phase synthesis method is 188-213, the dielectric loss is 0.00027-0.00031, and the dielectric temperature coefficient is -683ppm/DEG C-523ppm/DEG C. The niobium-magnesium-acid-bismuth based microwave dielectric ceramic material can be used for medium voltage controlled microwave devices in integrated circuits.
Description
Technical field
The present invention relates to microwave dielectric ceramic material manufacturing technology field, specifically magnoniobate bismuth base microwave dielectric ceramic material and preparation method.
Background technology
For adapting to the fast development of unicircuit, scientist has done number of research projects; In recent years, Bi cube of pyrochlore structure obtained research widely mutually, pottery with this phase structure has very high specific inductivity and dielectric tuning rate, in sizable test frequency scope, have low dielectric loss under the room temperature, and sintering temperature is also lower, and these performances make a Bi base cube pyrochlore structure pottery have application promise in clinical practice in multi-layer capacitor and integrated equipment.
As far back as the sixties in 20th century, Ba
xSr
1 xTiO
3(BST) the micro-wave dielectric tuning performance of ferroelectric material has just caused people's extensive interest.The characteristics of BST stupalith are dielectric tuning rate height, but dielectric loss is bigger, and relevant research is many; In recent years, discover that some bismuthino pyrochlore structure stupalith has higher dielectric tuning performance, dielectric loss is little, moderate specific inductivity, and temperature factor is little, is a kind of micro-wave dielectric material with adjustable that has development prospect.
Consist of Bi
1.5ZnNb
1.5O
7Bismuthino BZN material have pyrochlore structure, specific inductivity is moderate.But BZN stupalith tuning rate is low, reach certain tuning rate, and tuning electric field requires very high; With respect to the BZN stupalith, another one is matrix with the bismuth, have a cube pyrochlore structure, with the Bi of ternary system
2O
3-MgO-Nb
2O
5For the dielectric ceramic system on basis (being called for short BMN base pottery) begins to obtain to pay close attention in the embedded capacitor Application Areas, reason is exactly the high specific inductivity that has of this individual system and low dielectric loss; Studies show that compd B i
2Mg
2/3Nb
4/3O
7Specific inductivity very high, up to 210.And compd B i
2Zn
2/3Nb
4/3O
7Specific inductivity only be 86, the introducing of divalence magnesium ion may have been played the effect that strengthens dielectric response, the burnt green stone material of BMN bismuthino is a kind of very promising novel microwave dielectric material with adjustable.
The preparation method of microwave dielectric ceramic materials is a lot, synthesis by solid state reaction, hydrothermal synthesis method, chemical codeposition method (CVD), sol-gel method (Sol-gel) etc. are arranged, wherein adopt the maximum of solid-phase synthesis, the advantage of synthesis by solid state reaction is that method is simple to operation, and cost is lower.
Domestic and international many scholars are doing a lot of work aspect the preparation bismuthino dielectric ceramic material, main achievement is as follows: human metal organic deposit (MOD) methods such as the W.Ren of Pennsylvania State University have prepared the BZN film of cube phase at the Pt/Si substrate, have at first found the dielectric adjustable of BZN; People such as R.L.Thayer have found Bi in the process that is equipped with the BZN film with metal organic deposit (MOD) legal system
2O
3-ZnO-Nb
2O
5A kind of low temperature phase Bi in the system
1.5Zn
0.5Nb
1.5O
6.5, this low temperature is to obtain under annealing temperature is lower than 600 ℃ condition mutually, and cube pyrochlore constitution, specific inductivity are 180, and adjustable rate is 26%, 230ppm/ ℃ of temperature factor TCC Wei –; Human pulsed laser deposition (PLD) methods such as the S.W.Jiang of University of Electronic Science and Technology are at Pt/SiO
2Preparation BZN film on the/Si substrate, its adjustable rate is greater than 6%, and loss is lower than 0.004; Mg such as S.W.Jiang
2+Replace the Zn in the BZN material
2+Ion adopts the PLD method to prepare Bi
1.5MgNb
1.5O
7(BMN) the burnt green stone film of bismuthino, prepared BMN thin-film dielectric loss little (about 0.002), specific inductivity moderate (about 86) varies with temperature less (the about 500ppm/K of dielectric temperature coefficient T CC); People such as the neat blast of University of Electronic Science and Technology, Jiang Shuwen adopt the method for magnetron sputtering to prepare Bi
1.5ZnNb
1.5O
7(BZN) dielectric loss of the burnt green stone film of bismuthino is 0.002 ~ 0.004, and the dielectric tuning rate is about 20%; People such as AEHOON P, JIWEI W L discovers that also there is application in the BMN base ceramic material in phase shifter in addition; The present invention adopts solid-phase synthesis directly to prepare the micro-wave dielectric magnoniobate bismuthino stupalith that polycomponent mixes.
Summary of the invention
One of purpose of the present invention provides that a kind of product performance are good, production cost is low, method is simple, can be suitable for the microwave dielectric ceramic material of suitability for industrialized production.
Two of purpose of the present invention provides a kind of preparation method of magnoniobate bismuth base microwave dielectric ceramic material.
To achieve these goals, the present invention is by the following technical solutions:
A kind of Bi
1.5MgNb
1.5O
7The based microwave dielectric ceramics material is characterized in that: the component of described material by the mole percentage calculation is: Bi
2O
359%～60%, MgO6.9%～7.0%, Nb
2O
530%～33.2% is material of main part, Li
2CO
3, TiO
2Respectively be 0.15%～3%, be the dielectric function additive.
Described a kind of Bi
1.5MgNb
1.5O
7The based microwave dielectric ceramics preparation methods is characterized in that: utilize traditional solid-phase synthesis to prepare Bi
1.5MgNb
1.5O
7Based microwave dielectric ceramics material: prepare burden Bi according to following molar percentage component
2O
359%～60%, MgO6.9%～7.0%, Nb
2O
530%～33.2% is material of main part, Li
2CO
3, TiO
2Respectively be 0.15%～3% for the dielectric function additive; Adopt agate ball and stainless cylinder of steel, dehydrated alcohol is ball-milling medium, agate ball: the batching powder: the mass ratio of dehydrated alcohol is 2:1:1, and wet-milling 10h in planetary high-energy ball mill, rotating speed are 150rpm; The slurry that ball milling is good becomes dry powder at 70 ℃ of insulation 24 h; Adopt massfraction be 2% the PVA aqueous solution as binding agent, powder and PVA solution quality are crossed the accurate sub-sieve of 150 targets then than being 9:1, with 20MPa pressure pressurize 5min compacting, make powder become base; Base substrate is put into the Si-Mo rod high-temperature electric resistance furnace, rise to 950 ℃ with the speed of 3 ℃/min from room temperature, be incubated 150min in the air atmosphere, cool to room temperature with the furnace, finish the pre-burning to idiosome; After the pre-burning idiosome smashed and carry out secondary ball milling, the secondary ball milling parameter is identical with a ball milling, and the slurry that ball milling is good becomes dry powder at 70 ℃ of insulation 24 h; Adopt massfraction be 2% the PVA aqueous solution as binding agent, powder and PVA solution quality are crossed the accurate sub-sieve of 100 targets then than being 10:1, with 45MPa pressure pressurize 5min compacting, make powder become base; Base substrate is put into the Si-Mo rod high-temperature electric resistance furnace, rise to 550 ℃ with the speed of 1 ℃/min from room temperature, be incubated 300min in the air atmosphere, the back rises to 1130 ℃ of sintering temperatures with the speed of 2 ℃/min, is incubated 90min in the air atmosphere, cools to room temperature with the furnace.
After sintering is finished, to billet surface fine sandpaper sanding and polishing, guarantee that the base substrate two sides is smooth smooth, zero defect, then with ceramic body coated on both sides silver slurry, in drying baker in 70 ℃ of oven dry; Sample after the oven dry is put in the resistance furnace, rises to 600 ℃ by room temperature, insulation 30min forms silver electrode, namely gets magnoniobate bismuthino stupalith.
The present invention is by adjusting the rational proportion of dielectric function additive, and in conjunction with the magnoniobate bismuthino stupalith of preparation method's preparation, specific inductivity is 188～213, and dielectric loss is 0.00027～0.00031, and the dielectric temperature coefficient is-683ppm/ ℃ ~-523ppm/ ℃; Magnoniobate bismuth base microwave dielectric ceramic material of the present invention can be used for the voltage-controlled microwave device of unicircuit medium.
Technical superiority
1, preparation process is simple, and is repeatable higher, and cost is lower, is convenient to realize scale operation
2, by adjusting the ratio of dielectric function additive, BMN base ceramic material dielectric properties are greatly improved; Bao Dao Bi before
1.5MgNb
1.5O
7The dielectric ceramic material specific inductivity is about 86, and dielectric loss is less than 0.005, the dielectric temperature coefficient is-and 550ppm/ ℃; Contrast therewith, prepared ceramic dielectric loss is littler, and specific inductivity is improved, and the dielectric temperature coefficient is littler, and relaxation temperature can serve in the unicircuit BMN base ceramic material well below room temperature better.
Embodiment
After now embodiments of the invention being described in.
EXAMPLE l
1) utilize traditional solid-phase synthesis to prepare magnoniobate bismuth base microwave dielectric ceramic target: to prepare burden Bi according to following molar percentage component
2O
3: 59.0866%, MgO:6.931%, Nb
2O
5: 33.137%, Li
2CO
3: 0.1588%, TiO
2: 0.6866%.
2) adopt agate ball, stainless cylinder of steel, dehydrated alcohol is ball-milling medium, agate ball: batching powder: do not have
The mass ratio of water-ethanol is 2:1:1, and wet-milling 10h in planetary high-energy ball mill, rotating speed are 150rpm; The slurry that ball milling is good becomes dry powder at 70 ℃ of insulation 24 h; Adopt massfraction be 2% the PVA aqueous solution as binding agent, powder and PVA solution quality be than being 9:1, cross the accurate sub-sieve of 150 targets then after, with 20MPa pressure pressurize 5min compacting, make powder become base; Base substrate is put into the Si-Mo rod high-temperature electric resistance furnace, rise to 950 ℃ with the speed of 3 ℃/min from room temperature, be incubated 150min in the air atmosphere, cool to room temperature with the furnace, finish the pre-burning to idiosome.
3) after the pre-burning idiosome smashed and carry out secondary ball milling, the secondary ball milling parameter is identical with a ball milling; Ball
The slurry that mill is good becomes dry powder at 70 ℃ of insulation 24 h; Adopt massfraction be 2% the PVA aqueous solution as binding agent, powder and PVA solution quality are crossed the accurate sub-sieve of 100 targets then than being 10:1, with 45MPa pressure pressurize 5min compacting, make powder become base.
4) base substrate is put into the Si-Mo rod high-temperature electric resistance furnace, is risen to 550 ℃ with the speed of 1 ℃/min from room temperature,
Be incubated 300min in the air atmosphere, the back rises to 1130 ℃ of sintering temperatures with the speed of 2 ℃/min, is incubated 90min in the air atmosphere, cools to room temperature with the furnace.
5) to billet surface fine sandpaper sanding and polishing, guarantee that the base substrate two sides is smooth smooth, zero defect.{。##.##1},
After with ceramic body coated on both sides silver slurry, in drying baker in 70 ℃ of oven dry; Sample after the oven dry is put in the resistance furnace, rises to 600 ℃ by room temperature, insulation 30min forms silver electrode, namely gets magnoniobate bismuthino stupalith.
The magnoniobate bismuth base microwave dielectric ceramic material of present embodiment made is through performance test, and specific inductivity is 188.4959, and dielectric loss is 0.00030, and the dielectric temperature coefficient is-523ppm/ ℃.
Embodiment 2
In this example, prepare burden Bi according to following molar percentage component
2O
3: 59.358%, MgO:
6.9627%, Nb
2O
5: 32.1403%, Li
2CO
3: 0.1595%, TiO
2: 1.3795%, adopt the processing step identical with embodiment 1 to be made into magnoniobate bismuthino stupalith.
The magnoniobate bismuth base microwave dielectric ceramic film material of present embodiment made is through performance test, and specific inductivity is 198.6450, and dielectric loss is 0.00029, and the dielectric temperature coefficient is-621ppm/ ℃.
Embodiment 3
In this example, prepare burden Bi according to following molar percentage component
2O
3: 59.906%, MgO:
7.027%, Nb
2O
5: 30.121%, Li
2CO
3: 0.161%, TiO
2: 2.785%, adopt the processing step identical with embodiment 1 to be made into magnoniobate bismuthino stupalith.
The magnoniobate bismuth base microwave dielectric ceramic film material of present embodiment made is through performance test, and specific inductivity is 188.4959, and dielectric loss is 0.00027, and the dielectric temperature coefficient is-683ppm/ ℃.
Claims (3)
1. a magnoniobate bismuthino lithium titanium is replaced microwave dielectric ceramic material altogether, is Bi
1.5MgNb
1.5O
7The based microwave dielectric ceramics material is characterized in that: the component of described material by the mole percentage calculation is: Bi
2O
359%～60%, MgO6.9%～7.0%, Nb
2O
530%～33.2% is material of main part, Li
2CO
3, TiO
2Respectively be 0.15%～3%, be the dielectric function additive.
2. a kind of magnoniobate bismuthino lithium titanium as claimed in claim 1 is replaced microwave dielectric ceramic material altogether, it is characterized in that: the specific inductivity that described magnoniobate bismuthino lithium titanium is replaced microwave dielectric ceramic material altogether is 188～213, dielectric loss is 0.00027～0.00031, the dielectric temperature coefficient is-683ppm/ ℃ ~-523ppm/ ℃; Can be used for the voltage-controlled microwave device of unicircuit medium.
3. a kind of magnoniobate bismuthino lithium titanium as claimed in claim 1 is replaced the preparation method of microwave dielectric ceramic material altogether, it is characterized in that: utilize traditional solid-phase synthesis to prepare Bi
1.5MgNb
1.5O
7Based microwave dielectric ceramics material: prepare burden Bi according to following molar percentage component
2O
359%～60%, MgO6.9%～7.0%, Nb
2O
530%～33.2% is material of main part, Li
2CO
3, TiO
2Respectively be 0.15%～3%; Adopt agate ball and stainless cylinder of steel, dehydrated alcohol is ball-milling medium, agate ball: the batching powder: the mass ratio of dehydrated alcohol is 2:1:1, and wet-milling 10h in planetary high-energy ball mill, rotating speed are 150rpm; The slurry that ball milling is good becomes dry powder at 70 ℃ of insulation 24 h; Adopt massfraction be 2% the PVA aqueous solution as binding agent, powder and PVA solution quality are crossed the accurate sub-sieve of 150 targets then than being 9:1, with 20MPa pressure pressurize 5min compacting, make powder become base; Base substrate is put into the Si-Mo rod high-temperature electric resistance furnace, rise to 950 ℃ with the speed of 3 ℃/min from room temperature, be incubated 150min in the air atmosphere, cool to room temperature with the furnace, finish the pre-burning to idiosome; After the pre-burning idiosome smashed and carry out secondary ball milling, the secondary ball milling parameter is identical with a ball milling, and the slurry that ball milling is good becomes dry powder at 70 ℃ of insulation 24 h; Adopt massfraction be 2% the PVA aqueous solution as binding agent, powder and PVA solution quality are crossed the accurate sub-sieve of 100 targets then than being 10:1, with 45MPa pressure pressurize 5min compacting, make powder become base; Base substrate is put into the Si-Mo rod high-temperature electric resistance furnace, rise to 550 ℃ with the speed of 1 ℃/min from room temperature, be incubated 300min in the air atmosphere, the back rises to 1130 ℃ of sintering temperatures with the speed of 2 ℃/min, is incubated 90min in the air atmosphere, cools to room temperature with the furnace.
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Cited By (4)
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| CN103232239A (en) * | 2013-04-22 | 2013-08-07 | 江苏大学 | Microwave dielectric ceramic material and preparation method thereof |
| CN108929110A (en) * | 2018-08-13 | 2018-12-04 | 安徽长容电子有限公司 | A kind of high pressure resistant temperature-stable ceramic capacitor dielectric material and preparation method thereof |
| 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 |
| CN117153562A (en) * | 2023-09-19 | 2023-12-01 | 江苏飞特尔通信有限公司 | Bismuth-based adjustable MLCC capacitor for LTCC and preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103232239A (en) * | 2013-04-22 | 2013-08-07 | 江苏大学 | Microwave dielectric ceramic material and preparation method thereof |
| CN108929110A (en) * | 2018-08-13 | 2018-12-04 | 安徽长容电子有限公司 | A kind of high pressure resistant temperature-stable ceramic capacitor dielectric material and preparation method thereof |
| 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 |
| CN117153562A (en) * | 2023-09-19 | 2023-12-01 | 江苏飞特尔通信有限公司 | Bismuth-based adjustable MLCC capacitor for LTCC and preparation method |
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