CN102826847A - Composite high dielectric constant microwave dielectric ceramic material and preparation method thereof - Google Patents
Composite high dielectric constant microwave dielectric ceramic material and preparation method thereof Download PDFInfo
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- CN102826847A CN102826847A CN2012103516060A CN201210351606A CN102826847A CN 102826847 A CN102826847 A CN 102826847A CN 2012103516060 A CN2012103516060 A CN 2012103516060A CN 201210351606 A CN201210351606 A CN 201210351606A CN 102826847 A CN102826847 A CN 102826847A
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Abstract
The invention discloses a composite high dielectric constant microwave dielectric ceramic material and a preparation method of the material; the material comprises raw materials in the following molar ratio: 0.8 (Bi1.5MgNb1.5O7)-0.2 (beta-Bi2Zn2/3Nb4/3O7). The preparation method comprises the steps of: using a sol-gel method for pre-synthesizing Bi1.5MgNb1.5O7(BMN) and Bi2Zn2/3Nb4/3O7 (beta-BZN) nano ceramic powder, then mixing the pre-synthesized powder according to the molar ratio of 4: 1, adding 1.25% polyvinyl alcohol into the mixture and carrying out ball milling; drying, sieving, and molding by pressing; and sintering for 4h at the temperature of 960-1040 DEG C to obtain the composite high dielectric constant microwave dielectric ceramic material. The best dielectric constant and dielectric loss of the composite high dielectric constant microwave dielectric ceramic material are superior to those of the traditional BMN ceramics, so that the sintering temperature is lowered, the technical requirements of a low temperature co-fired ceramic (LTCC) system can be met, and the production cost is greatly reduced; and the obtained powder is uniform in composition and free from pollution in the process, and has wide application prospect.
Description
Technical field
The invention belongs to a kind of is the ceramic composition of characteristic with the composition, particularly a kind of low-temperature sintered microwave dielectric ceramic material and preparation method of Bi base composite high-dielectric constant.
Background technology
The low-temperature sintering microwave medium pottery is a research direction of dielectric substance aspect in recent years, also is the base mateiral of development chip multilayer microwave device.At present, the domestic and international research that reduces the microwave-medium ceramics sintering temperature is mainly concentrated on selects low melting component or eutectic as ceramic post sintering auxiliary agent aspect; Yet; Although different microwave-medium ceramics system is through doping low melting glass or oxide compound, its sintering temperature significantly reduces, because there is chemical reaction to take place between material principal crystalline phase and the glassy phase; Principal crystalline phase content is reduced; Or having impurity to produce mutually, its extrinsic loss (mainly being the mode of resonance vibration loss of glassy phase) increases, and makes the microwave dielectric property of material that decline in various degree also arranged.Therefore the microwave dielectric material of searching with sintering temperature and low itself becomes the focus of the concern field in.
Bi base Bi
2O
3-M
IIO-Nb
2O
5(BM
IIN, M
II=Zn is that ceramic intrinsic sintering temperature is low Mg), has relative higher dielectric constant, little dielectric loss and good microwave property, thereby has received widely and paying close attention to.
Bi
2O
3-ZnO-Nb
2O
5(BZN) basic ceramic sintering temperature is lower, can with the compatible MLC technology of Ag electrode; Yong et al. research shows that with change of component, there are two primary structure with different dielectric properties: Bi in BZN system pottery
1.5ZnNb
1.5O
7(α-BZN) green stone of cube Jiao and Bi
2Zn
2/3Nb
4/3O
7(the monocline titanium zirconium thorium structure of β _ BZN).Cube green stone Bi of Jiao
1.5ZnNb
1.5O
7(spacer of α-BZN) is Fd3m, the ε during 1MHz
r≈ 150, tan δ≤4 * 10
-4, τ
c≈-400 * 10
-6Bi
2Zn
2/3Nb
4/3O
7(spacer of β _ BZN) is C2/c, the ε during 1MHz
r≈ 80, tan δ≤2 * 10
-4, τ
C≈ 200 * 10
-6Although α-BZN pottery has excellent dielectric properties under low frequency; But see from result of study; When material structure is to contain the green stone phase time of cube Jiao; Loss is all very big under the microwave of sample, and this is relevant with the directric relaxation phenomenon that the BZN pottery is appeared, the following characteristics of directric relaxation tool in the green stone material of BZN base cube Jiao: the temperature T when maximum loss occurring
mWith test frequency increase shift to higher temperature, loss value with the increase of test frequency increase, the width and the height of loss peak increase with test frequency, the directric relaxation of this unusual broadband and TR causes the dielectric loss increase of material in the microwave frequency band room temperature.β _ BZN has good characteristic under microwave frequency band, when frequency is 3GHZ, and ε
r≈ 80, Q ≈ 1000, but its specific inductivity is less relatively.Therefore, can consider to optimize its microwave dielectric property with monocline is mutually compound through among the BZN cube, and two phase temperature factor opposite in signs, through Bi
1.5ZnNb
1.5O
7(α-BZN) and Bi
2Zn
2/3Nb
4/3O
7(β _ BZN) compound can realize zero-temperature coefficient, but experiment shows that α _ BZN and β _ BZN are compound, and microwave dielectric property lifting to material is limited, and the specific inductivity of matrix material is less relatively.
Bi
2O
3-MgO-Nb
2O
5(BMN) the green feldspar material B of base cube Jiao i
1.5MgNb
1.5O
7The performance performance is excellent: high specific inductivity (ε
r>=150), low-dielectric loss (tan δ≤4 * 10
-4) and the temperature factor adjustable, but its sintering temperature is higher relatively, generally greater than 1100 ℃; It should be noted that with respect to Bi
2Zn
2/3Nb
4/3O
7(β _ BZN), Bi
2Mg
2/3Nb
4/3O
7Specific inductivity is higher, the ε during 1MHz
r≈ 210, and this phenomenon shows, Mg
2+Introducing can promote the dielectric response of system to a great extent.Therefore, the advantage of comprehensive BMN and BZN ceramic systems is chosen Bi
1.5MgNb
1.5O
7With Bi
2Zn
2/3Nb
4/3O
7It is compound that two kinds of potteries carry out, and is expected to obtain high-k, low-loss low-temperature sintered microwave dielectric ceramic material.
Simultaneously, we notice when research Bi sill structure and performance, are to be equipped with sample with the conventional solid state reaction legal system basically.Compare with conventional solid-state method, wet chemistry method is an origin with homogeneous, stable solution, makes solute and separated from solvent by all means, perhaps impels it that chemical reaction takes place, and the presoma of the required powder that forms at last obtains expecting powder after the thermal treatment.This class methods cost is low, the component easy-regulating, make things convenient for novel material trial-production.Can comparatively fast obtain new texture, new component stupalith powder in this method aspect the preparation doped samples.Wang etc. are with Bi (OOCCH
3)
3, Zn (OOCCH
3)
2, Nb (OCH
2CH
3)
5Be raw material, adopt metallorganics thermolysis (MOD) method to prepare even and fine α-BZN powder, the grain-size of 800 ℃ of sintered samples is between 200~500nm.Compare with traditional solid phase preparation technology, the BZN pottery of MOD method preparation, sintering temperature reduces, and grain-size reduces, the ε of 900 ℃ of sintered samples
r≈ 142, tan δ ≈ 3 * 10
-4, τ
c≈ – 480 * 10
-6/ ℃.Adopt Bi (NO
3)
3XH
2O, Mg (NO
3)
36H
2O, Nb (OCH
3)
5Be raw material, with metal citrate method low temperature synthetic Bi
2O
3-MgO-Nb
2O
5Nano-powder can obtain single-phase cube of pyrochlore structure through handling more than 500 ℃.Obtain the equally distributed spherical powder of 16nm at 600 ℃, can obtain the sample of high densification, uniform microstructure through 850 ℃ of discharge plasma sinterings.But from economic angle, because the alkoxide (Nb (OCH of Nb
2CH
3)
5, Nb (OCH
3)
5)) cost an arm and a leg, and volatilization easily, the preparation process is not easy to operate, and therefore above two kinds of methods are not suitable for large-scale industrial production.
Summary of the invention
The object of the invention provides a kind of Bi base composite high-dielectric constant low temperature sintered microwave dielectric material and preparation method that can reduce sintering temperature, also not make the decline of specific inductivity simultaneously.
The present invention is achieved through following technical scheme.
A kind of composite high-dielectric constant microwave dielectric ceramic materials, chemical formula is Bi
1.5MgNb
1.5O
7-β _ Bi
2Zn
2/3Nb
4/3O
7, mol ratio is 0.8:0.2.
The preparation method of composite high-dielectric constant microwave dielectric ceramic materials has following steps:
(1) the synthetic in advance Bi of sol-gel method
1.5MgNb
1.5O
7Abbreviate BMN and Bi as
2Zn
2/3Nb
4/3O
7Abbreviate β _ BZN nano-ceramic powder as
1. prepare the aqueous citric acid solution of niobium
(a) stoichiometric ratio according to BMN and β _ BZN takes by weighing Nb
2O
5, with Nb
2O
5Put into two parts of hydrofluoric acid respectively, heating in water bath is to Nb
2O
5All dissolvings;
(b) in above-mentioned two parts of solution, add ammoniacal liquor, generate the niobic acid deposition;
(c) the above-mentioned two parts of depositions of filtering and washing add niobic acid respectively in the lemon aqueous acid then, obtain the aqueous citric acid solution of niobium, and wherein the mol ratio of niobium ion and Hydrocerol A is 1:6;
Add terepthaloyl moietie in the aqueous citric acid solution of the niobium that 2. 1. step is made, heated and stirred, the mole of Hydrocerol A and terepthaloyl moietie is 1:3;
3. prepare Mg respectively
2+, Zn
2+With Bi
3+Ethylene glycol solution
(a) take by weighing five water Bismuth trinitrates by stoichiometric ratio, magnesium nitrate hexahydrate is dissolved in terepthaloyl moietie and stirs;
(b) take by weighing five water Bismuth trinitrates by stoichiometric ratio, zinc nitrate hexahydrate is dissolved in terepthaloyl moietie and stirs;
4. the formation of the formation of bismuth magnesium niobium, bismuth zinc niobium colloidal sol and niobic acid bismuth magnesium, bismuthic acid zinc niobium nano-powder
(a) with step 3. (a), 3. (b) configuration Bi
3+Ethylene glycol solution and Mg
2+, Zn
2+Ethylene glycol solution add in the liquid that 2. step dispose, stirring obtains bismuth magnesium niobium colloidal sol, bismuth zinc niobium colloidal sol;
(b) colloidal sol with step (a) places baking oven, in 80 ~ 120 ℃ of oven dry, forms xerogel;
(c) xerogel with step (b) places High Temperature Furnaces Heating Apparatus, obtains niobic acid bismuth magnesium, bismuthic acid zinc niobium nano-powder in 550 ~ 750 ℃ of thermal treatments;
(2) the niobic acid bismuth magnesium that step (1) is configured, bismuthic acid zinc niobium nano-ceramic powder 4:1 in molar ratio mix, and add 1.25% Z 150PH, put into ball grinder, add zirconia ball and deionized water, ball milling 6 hours;
(3) raw material behind step (2) ball milling is dried in infrared drying oven, sieve; Use powder compressing machine to be pressed into base substrate again with the pressure of 4 ~ 6MPa.
(4) with the base substrate of step (3) in 960 ~ 1040 ℃ of sintering 4 hours, process composite high-dielectric constant microwave dielectric ceramic materials;
(5) microwave dielectric property of test article.
The mass ratio of the nano-ceramic powder of said step (2) and zirconia ball, deionized water is 1: 1: 2.
The base substrate of said step (3) is the disk of Φ 10mm * 5mm.
The preferred sintering temperature of said step (3).
Sol-gel method is adopted in ceramic powder preparation of the present invention, with Bi (NO
3)
36H
2O, Mg (NO
3)
36H
2O, Nb
2O
5Be raw material, make 0.8BMN-0.2 β _ BZN composite high dielectric constant low-temperature sintered microwave dielectric ceramic material, its sintering temperature is 960 ~ 1040 ℃, DIELECTRIC CONSTANTS
r>=140, dielectric loss tan δ≤2.3 * 10
-4, temperature coefficient of capacitance τ
C≈-400 * 10
-6Each item index is all close with traditional B MN pottery, and best specific inductivity and dielectric loss are superior to the BMN pottery, have both reduced sintering temperature, has satisfied the requirement of LTCC system (LTCC) technology again.In addition, reduced production cost significantly, easy to operation, can satisfy industrial requirement; The powder component homogeneous that this preparation technology obtains, process is pollution-free, has broad application prospects.
Embodiment
The raw materials used AR that is of the present invention, specific embodiment is following.
Embodiment 1
(1) the synthetic in advance Bi of sol-gel method
1.5MgNb
1.5O
7(BMN) and Bi
2Zn
2/3Nb
4/3O
7(nano-ceramic powder of β _ BZN), its proportioning raw materials is as shown in table 1;
Table 1
The practical implementation step is following:
1. prepare the aqueous citric acid solution of niobium
(a) according to Bi
1.5MgNb
1.5O
7With β _ Bi
2Zn
2/3Nb
4/3O
7Stoichiometric ratio take by weighing Nb
2O
5, with Nb
2O
5Put into two parts of hydrofluoric acid respectively, heating in water bath is to Nb
2O
5All dissolvings;
(b) in above-mentioned two parts of solution, add ammoniacal liquor, generate the niobic acid deposition;
(c) the above-mentioned deposition of filtering and washing adds niobic acid in the lemon aqueous acid then, obtains the aqueous citric acid solution of niobium, and wherein the mol ratio of niobium ion and Hydrocerol A is 1:6;
Add terepthaloyl moietie in the aqueous citric acid solution of the niobium that 2. 1. step is made, heated and stirred, the mole of Hydrocerol A and terepthaloyl moietie is 1:3;
3. prepare Mg respectively
2+, Zn
2+With Bi
3+Ethylene glycol solution
(a) take by weighing five water Bismuth trinitrates by stoichiometric ratio, magnesium nitrate hexahydrate is dissolved in terepthaloyl moietie and stirs;
(b) take by weighing five water Bismuth trinitrates by stoichiometric ratio, zinc nitrate hexahydrate is dissolved in terepthaloyl moietie and stirs;
4. the formation of the formation of bismuth magnesium niobium, bismuth zinc niobium colloidal sol and niobic acid bismuth magnesium, bismuthic acid zinc niobium nano-powder
(a) with step 3. (a), 3. (b) configuration Bi
3+Ethylene glycol solution and Mg
2+, Zn
2+Ethylene glycol solution add step
2. in the liquid of configuration, stirring obtains bismuth magnesium niobium colloidal sol, bismuth zinc niobium colloidal sol;
(b) colloidal sol with step (a) places baking oven, in 80 ~ 120 ℃ of oven dry, forms xerogel;
(c) xerogel with step (b) places High Temperature Furnaces Heating Apparatus, obtains niobic acid bismuth magnesium, bismuthic acid zinc niobium nano-powder in 550 ~ 750 ℃ of thermal treatments;
(3) the nano-ceramic powder Bi that step (1) is configured
1.5MgNb
1.5O
7(BMN) and Bi
2Zn
2/3Nb
4/3O
7(β _ BZN) 4:1 mixes in molar ratio, adds 1.25% Z 150PH, puts into ball grinder, adds zirconia ball and deionized water, ball milling 6 hours
(3) raw material behind the ball milling is dried in infrared drying oven, sieve; Use powder compressing machine to be pressed into the disk of Φ 10mm * 1mm with the pressure of 4 ~ 6MPa again.
(4) with disk in 960 ℃ of sintering 4 hours.
(5) adopt its microwave dielectric property of Agilent 4278A electric impedance analyzer test, under the 1MHz, ε
r=140.2, tan δ=1.9 * 10
-4, τ
C=-400 * 10
-6
Embodiment 2-5
Sintering temperature and the microwave dielectric property of embodiment 2-5 see table 2 for details, and all the other preparation processes and embodiment 1 are identical.
Table 2
Claims (5)
1. composite high-dielectric constant microwave dielectric ceramic materials, chemical formula is Bi
1.5MgNb
1.5O
7-β _ Bi
2Zn
2/3Nb
4/3O
7, mol ratio is 0.8:0.2.
2. the preparation method of the composite high-dielectric constant microwave dielectric ceramic materials of claim 1 has following steps:
(1) the synthetic in advance Bi of sol-gel method
1.5MgNb
1.5O
7Abbreviate BMN and Bi as
2Zn
2/3Nb
4/3O
7Abbreviate β _ BZN nano-ceramic powder as
1. prepare the aqueous citric acid solution of niobium
(a) stoichiometric ratio according to BMN and β _ BZN takes by weighing Nb
2O
5, with Nb
2O
5Put into two parts of hydrofluoric acid respectively, heating in water bath is to Nb
2O
5All dissolvings;
(b) in above-mentioned two parts of solution, add ammoniacal liquor, generate the niobic acid deposition;
(c) the above-mentioned two parts of depositions of filtering and washing add niobic acid respectively in the lemon aqueous acid then, obtain the aqueous citric acid solution of niobium, and wherein the mol ratio of niobium ion and Hydrocerol A is 1:6;
Add terepthaloyl moietie in the aqueous citric acid solution of the niobium that 2. 1. step is made, heated and stirred, the mole of Hydrocerol A and terepthaloyl moietie is 1:3;
3. prepare Mg respectively
2+, Zn
2+With Bi
3+Ethylene glycol solution
(a) take by weighing five water Bismuth trinitrates by stoichiometric ratio, magnesium nitrate hexahydrate is dissolved in terepthaloyl moietie and stirs;
(b) take by weighing five water Bismuth trinitrates by stoichiometric ratio, zinc nitrate hexahydrate is dissolved in terepthaloyl moietie and stirs;
4. the formation of the formation of bismuth magnesium niobium, bismuth zinc niobium colloidal sol and niobic acid bismuth magnesium, bismuthic acid zinc niobium nano-powder
(a) with step 3. (a), 3. (b) configuration Bi
3+Ethylene glycol solution and Mg
2+, Zn
2+Ethylene glycol solution add in the liquid that 2. step dispose, stirring obtains bismuth magnesium niobium colloidal sol, bismuth zinc niobium colloidal sol;
(b) colloidal sol with step (a) places baking oven, in 80 ~ 120 ℃ of oven dry, forms xerogel;
(c) xerogel with step (b) places High Temperature Furnaces Heating Apparatus, obtains niobic acid bismuth magnesium, bismuthic acid zinc niobium nano-powder in 550 ~ 750 ℃ of thermal treatments;
(2) the niobic acid bismuth magnesium that step (1) is configured, bismuthic acid zinc niobium nano-ceramic powder 4:1 in molar ratio mix, and add 1.25% Z 150PH, put into ball grinder, add zirconia ball and deionized water, ball milling 6 hours;
(3) raw material behind step (2) ball milling is dried in infrared drying oven, sieve; Use powder compressing machine to be pressed into base substrate again with the pressure of 4 ~ 6MPa.
(4) with the base substrate of step (3) in 960 ~ 1040 ℃ of sintering 4 hours, process composite high-dielectric constant microwave dielectric ceramic materials;
(5) microwave dielectric property of test article.
3. according to the preparation method of the composite high-dielectric constant microwave dielectric ceramic materials of claim 2, it is characterized in that the mass ratio of the nano-ceramic powder of said step (2) and zirconia ball, deionized water is 1: 1: 2.
4. according to the preparation method of the composite high-dielectric constant microwave dielectric ceramic materials of claim 2, it is characterized in that the base substrate of said step (3) is the disk of Φ 10mm * 5mm.
5. according to the preparation method of the composite high-dielectric constant microwave dielectric ceramic materials of claim 2, it is characterized in that the preferred sintering temperature of said step (3).
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CN103467097A (en) * | 2013-08-29 | 2013-12-25 | 中国人民解放军国防科学技术大学 | Temperature-stable microwave dielectric ceramic with high dielectric constant and preparation method of microwave dielectric ceramic |
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CN103864427A (en) * | 2014-02-27 | 2014-06-18 | 天津大学 | Low-temperature sintering temperature-stabilizing type high-frequency dielectric ceramic and preparation method thereof |
CN110330330A (en) * | 2019-07-12 | 2019-10-15 | 无锡工艺职业技术学院 | A kind of microwave dielectric ceramic material and preparation method thereof with high magnetic permeability |
CN110436894A (en) * | 2019-06-27 | 2019-11-12 | 深圳顺络电子股份有限公司 | A kind of low-k LTCC material and preparation method thereof |
CN111689776A (en) * | 2019-03-15 | 2020-09-22 | Tdk株式会社 | Dielectric composition and electronic component |
CN111876756A (en) * | 2020-07-15 | 2020-11-03 | 齐鲁工业大学 | BMN multilayer dielectric film and preparation method thereof |
RU2804938C1 (en) * | 2023-04-13 | 2023-10-09 | Федеральное государственное автономное учреждение высшего образования "Южный федеральный университет" | Method for producing ceramic material based on bismuth-zinc-niobium oxides |
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