CN103936411A - Method for preparing ultra-wide temperature stable barium titanate dielectric material by adopting annealing method - Google Patents

Method for preparing ultra-wide temperature stable barium titanate dielectric material by adopting annealing method Download PDF

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CN103936411A
CN103936411A CN201410134314.0A CN201410134314A CN103936411A CN 103936411 A CN103936411 A CN 103936411A CN 201410134314 A CN201410134314 A CN 201410134314A CN 103936411 A CN103936411 A CN 103936411A
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dielectric material
tio
base dielectric
ball milling
wide temperature
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CN103936411B (en
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李玲霞
陈俊晓
张宁
柳亚然
高正东
于经洋
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Tianjin University
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Abstract

The invention discloses a method for preparing an ultra-wide temperature stable barium titanate dielectric material by adopting an annealing method. The method comprises the following step: annealing a barium titanate dielectric material obtained by the traditional solid-phase process method at 1,000-1100 DEG C for 1-8 hours to finally obtain the ultra-wide temperature stable barium titanate dielectric material with excellent performance. The stability of the dielectric constant of the barium titanate dielectric material and the dielectric constant of a high-temperature section (150-310 DEG C) is significantly improved; the method has excellent dielectric properties, wherein epsilon r is greater than or equal to 1600, the insulation resistivity is greater than 10<11>ohm.cm, the rate of change of capacitance within a range of -55 DEG C to 310 DEG C, namely delta C/C at 20 DEG C is smaller than or equal to +/-15%, and tan delta is smaller than or equal to 2%.

Description

Adopt annealing method to prepare the method for super wide temperature stable form barium phthalate base dielectric material
Technical field
The invention belongs to a kind of ceramic composition taking composition as feature, particularly a kind of method that adopts annealing method to prepare super wide temperature stable form barium phthalate base dielectric material.
Background technology
Along with the high speed development of multiple mobile electronic device such as notebook computer, mobile telephone, digital camera, automotive electronics etc., chip electronic component has progressively replaced conventional wire type electronic component.Chip multilayer ceramic capacitor (MLCC) is the chip components and parts of current turnout, sales volume maximum, and it is electrode materials and ceramic body to be replaced to parallel connection with multilayer be superimposed together, and burns till an entirety simultaneously.
In recent years, MLCC is to improve its over-all properties by the development trend of dielectric material always, ensureing under the prerequisite of its high reliability, expand its use temperature scope, successively there is meeting EIA(Electronic Industries Associate, international Electronic Industries Association USA) X7R(operating temperature range be-55～125 DEG C), X8R(operating temperature range is-55～150 DEG C), X9R(operating temperature range is-55～200 DEG C) dielectric material of standard.But, in fields such as aerospace, geological prospecting, automotive electronics, the environment for use of MLCC is harsher, X9R cannot meet service requirements completely, therefore improve the dielectric temperature stability of barium phthalate base dielectric material and obtain large as far as possible operation temperature area and remain one of current study hotspot, and now the research emphasis of dielectric capacitor manufacturer around formula and preparation technology's research.
Summary of the invention
Object of the present invention, is to provide a kind of method of being improved and obtained super wide temperature stable form barium phthalate base dielectric material by annealing method.Can anneal by the barium phthalate base dielectric material that traditional liquid process method is obtained, finally obtain super wide temperature stable form barium phthalate base dielectric material.
Adopt annealing method to prepare a method for super wide temperature stable form barium phthalate base dielectric material, step is as follows:
(1) by Na 2cO 3, Bi 2o 3, TiO 2by mole% 1:1:4 batching, with deionized water mixing and ball milling 4h post-drying and in 800 DEG C of calcinings, make Na 0.5bi 0.5tiO 3solid particulate;
(2) by Na 0.5bi 0.5tiO 3, BaTiO 3, Nb 2o 51:6.2:0.17 batching, with deionized water mixing and ball milling 4h post-drying and in 1000 DEG C of pre-burnings, makes frit in mass ratio;
(3) to the glass powder of additional mass percent 5% again in step (2) pre-burning gained frit, and the mass percent magnesium oxide that is 1.5% and the mass percent cerium oxide that is 0.3%, then in deionized water ball milling 2h, dry;
(4) step (3) is dried to the paraffin granulation that in gained powder, additional mass percent is 5～8%, then cross 1000 holes/cm 3sub-sieve, then be pressed into green compact, forming pressure 6～10MPa;
(5) step (4) gained green compact are used to the mode sintering that buries material, be first warming up to 550 DEG C of de-waxings through 3.5h, then rise to 1120 DEG C of sintering through 1.5h, insulation 1h, makes barium phthalate base dielectric material;
(6) step (5) gained barium phthalate base dielectric material is carried out to anneal, 1000 DEG C～1100 DEG C of annealing temperatures, annealing time 1～8h, finally obtains the super wide temperature stable form barium phthalate base dielectric material of excellent performance.
Described step (1), (2), (3) are all used QM-3SP4 planetary ball mill to carry out ball milling, 400 revs/min of drum'ss speed of rotation.
Glass powder composition and the mass percentage content of described step (3) are: 20%Bi 2o 3, 30%Pb 3o 4, 30%TiO 2, 20%H 3bO 3.
Described step (4) adopts 769YP-24B type powder compressing machine to be pressed, and uses Φ 20 moulds.
Method for annealing of the present invention can significantly improve the stability of specific inductivity and high temperature section (150 DEG C-310 DEG C) specific inductivity of dielectric material, and the final barium phthalate base dielectric material obtaining has excellent dielectric properties (ε r>=1600, insulation resistivity is greater than 10 11Ω cm, rate of change of capacitance Δ C/C within the scope of-55 DEG C～310 DEG C 20 DEG C≤ ± 15%, tan δ≤2%), 1000 DEG C～1100 DEG C of its annealing temperatures.
Embodiment
The raw materials used analytical pure raw material that all adopts of the present invention, specific embodiment is as follows.
Embodiment 1:
First by Na 2cO 3, Bi 2o 3, TiO 2by matter molar percentage 1:1:4 batching, with deionized water mixing and ball milling, use QM-3SP4 planetary ball mill (400 revs/min of drum'ss speed of rotation) ball milling 4h post-drying and in 800 DEG C of pre-burnings, make Na 0.5bi 0.5tiO 3solid particulate; By Na 0.5bi 0.5tiO 3, BaTiO 3, Nb 2o 5be in mass ratio: Na 0.5bi 0.5tiO 3: BaTiO 3: Nb 2o 5=1:6.2:0.17 batching, with deionized water mixing and ball milling, is used QM-3SP4 planetary ball mill (400 revs/min of drum'ss speed of rotation) ball milling 4h post-drying and in 1000 DEG C of pre-burnings, makes frit; To the glass powder of additional mass percent 5% in pre-burning gained frit, (glass powder composition and mass percentage content thereof are: 20%Bi 2o 3, 30%Pb 3o 4, 30%TiO 2, 20%H 3bO 3), and the cerium oxide of the magnesium oxide of mass percent 1.5% and mass percent 0.3%, mixing and ball milling in deionized water, is used QM-3SP4 planetary ball mill (400 revs/min of drum'ss speed of rotation) ball milling 2h, dries.Gained being dried to powder China and foreign countries, to add mass percent be 5% paraffin granulation again, then crosses 1000 holes/cm 3sub-sieve, uses Φ 20 moulds, on 769YP-24B type powder compressing machine, is pressed into green compact, forming pressure 6MPa.When sintering, be first warming up to 550 DEG C of de-waxings through 3h, then rise to 1120 DEG C of sintering through 1.5h, insulation 1h, makes barium phthalate base dielectric material.The gained barium phthalate base dielectric material 1h that anneals at 1000 DEG C just again, finally obtains the super wide temperature stable form barium phthalate base dielectric material of excellent performance.Again the upper and lower surface of resulting product is evenly applied to silver slurry, prepare electrode through 840 DEG C of burning infiltrations, make the ceramic condenser of wide operating temperature range.
Embodiment 2:
First by Na 2cO 3, Bi 2o 3, TiO 2by matter molar percentage 1:1:4 batching, with deionized water mixing and ball milling, use QM-3SP4 planetary ball mill (400 revs/min of drum'ss speed of rotation) ball milling 4h post-drying and in 800 DEG C of pre-burnings, make Na 0.5bi 0.5tiO 3solid particulate; By Na 0.5bi 0.5tiO 3, BaTiO 3, Nb 2o 5be in mass ratio: Na 0.5bi 0.5tiO 3: BaTiO 3: Nb 2o 5=1:6.2:0.17 batching, with deionized water mixing and ball milling, is used QM-3SP4 planetary ball mill (400 revs/min of drum'ss speed of rotation) ball milling 4h post-drying and in 1000 DEG C of pre-burnings, makes frit; (glass powder composition and mass percentage content thereof are the glass powder that is 5% to additional mass percent in pre-burning gained frit: 20%Bi 2o 3, 30%Pb 3o 4, 30%TiO 2, 20%H 3bO 3), and the mass percent magnesium oxide that is 1.5% and the mass percent cerium oxide that is 0.3%, mixing and ball milling in deionized water, is used QM-3SP4 planetary ball mill (400 revs/min of drum'ss speed of rotation) ball milling 2h, dries.Again gained is dried in powder, to add mass percent be 5% paraffin granulation, then cross 1000 holes/cm 3sub-sieve, uses Φ 20 moulds, on 769YP-24B type powder compressing machine, is pressed into green compact, forming pressure 6MPa.When sintering, be first warming up to 550 DEG C of de-waxings through 3h, then rise to 1120 DEG C of sintering through 1.5h, insulation 1h, makes barium phthalate base dielectric material.By the gained barium phthalate base dielectric material 3h that anneals, finally obtain the super wide temperature stable form barium phthalate base dielectric material of excellent performance at 1050 DEG C.Again the upper and lower surface of resulting product is evenly applied to silver slurry, prepare electrode through 840 DEG C of burning infiltrations, make the ceramic condenser of wide operating temperature range.
Embodiment 3:
First by Na 2cO 3, Bi 2o 3, TiO 2by matter molar percentage 1:1:4 batching, with deionized water mixing and ball milling, use QM-3SP4 planetary ball mill (400 revs/min of drum'ss speed of rotation) ball milling 4h post-drying and in 800 DEG C of pre-burnings, make Na 0.5bi 0.5tiO 3solid particulate; By Na 0.5bi 0.5tiO 3, BaTiO 3, Nb 2o 5be in mass ratio: Na 0.5bi 0.5tiO 3: BaTiO 3: Nb 2o 5=1:6.2:0.17 batching, with deionized water mixing and ball milling, is used QM-3SP4 planetary ball mill (400 revs/min of drum'ss speed of rotation) ball milling 4h post-drying and in 1000 DEG C of pre-burnings, makes frit; To the glass powder of additional mass percent 5% in pre-burning gained frit, (glass powder composition and mass percentage content thereof are: 20%Bi 2o 3, 30%Pb 3o 4, 30%TiO 2, 20%H 3bO 3), and the cerium oxide of the magnesium oxide of mass percent 1.5% and mass percent 0.3%, mixing and ball milling in deionized water, is used QM-3SP4 planetary ball mill (400 revs/min of drum'ss speed of rotation) ball milling 2h, dries.Again gained is dried in powder, to add mass percent be 5% paraffin granulation, then cross 1000 holes/cm 3sub-sieve, uses Φ 20 moulds, on 769YP-24B type powder compressing machine, is pressed into green compact, forming pressure 6MPa.When sintering, be first warming up to 550 DEG C of de-waxings through 3h, then rise to respectively 1120 DEG C of sintering through 1.5h, insulation 1h, makes barium phthalate base dielectric material.By the gained barium phthalate base dielectric material 8h that anneals, finally obtain the super wide temperature stable form barium phthalate base dielectric material of excellent performance at 1100 DEG C.Again the upper and lower surface of resulting product is evenly applied to silver slurry, prepare electrode through 840 DEG C of burning infiltrations, make the ceramic condenser of wide operating temperature range.
Testing method of the present invention and test set are as follows: (AC test signals: frequency is 1kHz, voltage is 1V).
(1) test of specific inductivity and loss (20 DEG C of room temperatures)
Use electrical capacity C and the loss tan δ of HEWLETT PACKARD4278A type capacitance tester test sample, and converse the specific inductivity of sample.For wafer capacitance device, conversion relation is as follows:
&epsiv; = 14.4 &times; c &times; d D 2
In formula: C-electrical capacity, unit is pF; D, D are respectively thickness, the diameter of sample, the cm of unit.
(2) test of resistivity
Use the insulation resistance Ri of Agilent4339B megger test sample, and converse the insulation resistivity ρ v of sample, as follows for wafer type sample reduction formula:
&rho; v = R i &times; &pi; &times; D 2 4 d
In formula: the volume specific resistance that ρ v is sample, unit is Ω cm; Ri is the insulation resistance of sample, and unit is Ω; D, D are respectively thickness, the diameter of sample, and unit is cm.
(3) TC characteristic test
Measure sample in warm area-55 DEG C～electrical capacity of+310 DEG C.Then adopt following formula rated capacity rate of temperature change:
&Delta;C C = C 2 - C 1 C 1 &times; 100 %
In formula: C1 is the electrical capacity at 20 DEG C, nF; C2 is the electrical capacity of arbitrary temp point in-55 DEG C～310 DEG C warm areas, nF; Δ C/C 20for the relative change rate of electrical capacity.
Experiment utilizes GZ-ESPEK high-low temperature chamber and STH-120 type high-temperature cabinet jointly to create the probe temperature environment of-55 DEG C～+ 310 DEG C, and adopts HM27002 type electrical condenser C-T/V characteristic dedicated tester and HEWLETT PACKARD4278A test to show.HM27002 type electrical condenser C-T/V characteristic dedicated tester is set to " interior inclined to one side ", starts to test, then rise to 20 DEG C of room temperatures from-55 DEG C, finally rises to+310 DEG C the electrical capacity by 4278A type capacitance measuring tester measure sample in whole warm area.
The main technologic parameters of above-described embodiment and dielectric properties test result refer to table 1.
Max| Δ C/C in table 1 20 DEG C| (%) the warm area scope of value is-55 DEG C～+ 310 DEG C.
Table 1
Adopt conventional solid-state method and do not pass through the same formula dielectric material of anneal, its specific inductivity is lower than 1500, and in the broad warm area of 150 DEG C～310 DEG C, variation of capacitance with temperature is excessive, cannot meet Δ C/C 20dEG C≤± 15%.The super wide temperature stable form barium phthalate base dielectric material that the application's method for annealing obtains, its annealing temperature is: 1000～1100 DEG C, annealing time 1～8h, operating temperature range is-55 DEG C～+ 310 DEG C and meets following dielectric properties:
Specific inductivity: ε >=1600, maximum dielectric constant ε=1939;
Loss: tan δ≤2.0%;
Temperature profile: Δ C/C 20dEG C≤± 15%.

Claims (4)

1. adopt annealing method to prepare a method for super wide temperature stable form barium phthalate base dielectric material, step is as follows:
(1) by Na 2cO 3, Bi 2o 3, TiO 2by mole% 1:1:4 batching, with deionized water mixing and ball milling 4h post-drying and in 800 DEG C of calcinings, make Na 0.5bi 0.5tiO 3solid particulate;
(2) by Na 0.5bi 0.5tiO 3, BaTiO 3, Nb 2o 51:6.2:0.17 batching, with deionized water mixing and ball milling 4h post-drying and in 1000 DEG C of pre-burnings, makes frit in mass ratio;
(3) to the glass powder of additional mass percent 5% again in step (2) pre-burning gained frit, and the mass percent magnesium oxide that is 1.5% and the mass percent cerium oxide that is 0.3%, then in deionized water ball milling 2h, dry;
(4) step (3) is dried to the paraffin granulation that in gained powder, additional mass percent is 5～8%, then cross 1000 holes/cm 3sub-sieve, then be pressed into green compact, forming pressure 6～10MPa;
(5) step (4) gained green compact are used to the mode sintering that buries material, be first warming up to 550 DEG C of de-waxings through 3.5h, then rise to 1120 DEG C of sintering through 1.5h, insulation 1h, makes barium phthalate base dielectric material;
(6) step (5) gained barium phthalate base dielectric material is carried out to anneal, 1000 DEG C～1100 DEG C of annealing temperatures, annealing time 1～8h, finally obtains the super wide temperature stable form barium phthalate base dielectric material of excellent performance.
2. employing annealing method according to claim 1 is prepared the method for super wide temperature stable form barium phthalate base dielectric material, it is characterized in that, described step (1), (2), (3) are all used QM-3SP4 planetary ball mill to carry out ball milling, 400 revs/min of drum'ss speed of rotation.
3. the wide operating temperature range medium material for multilayer ceramic capacitors of one according to claim 1, is characterized in that, glass powder composition and the mass percentage content of described step (3) are: 20%Bi 2o 3, 30%Pb 3o 4, 30%TiO 2, 20%H 3bO 3.
4. the wide operating temperature range medium material for multilayer ceramic capacitors of one according to claim 1, is characterized in that, described step (4) adopts 769YP-24B type powder compressing machine to be pressed, and uses Φ 20 moulds.
CN201410134314.0A 2014-04-03 2014-04-03 Use the method that annealing method prepares ultra-wide temperature stable type barium phthalate base dielectric material Expired - Fee Related CN103936411B (en)

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CN106116567A (en) * 2016-06-22 2016-11-16 刘和来 The preparation method of high density nano barium titanate titanate ceramics
CN110078495A (en) * 2019-04-25 2019-08-02 北京元六鸿远电子科技股份有限公司 The adjustable wide temperature range medium ceramic material of dielectric constant
CN110577401A (en) * 2019-08-14 2019-12-17 天津大学 preparation method of titanium dioxide-based dielectric material
CN113880573A (en) * 2021-09-10 2022-01-04 天津大学 Temperature-stable low-dielectric-loss microwave dielectric ceramic material and preparation method thereof
CN114853468A (en) * 2022-03-23 2022-08-05 哈尔滨理工大学 High-dielectric low-loss doped barium calcium titanate ceramic and preparation method thereof
CN114940616A (en) * 2022-04-08 2022-08-26 桂林理工大学 Rare earth modified strontium titanate giant dielectric ceramic material and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106116567A (en) * 2016-06-22 2016-11-16 刘和来 The preparation method of high density nano barium titanate titanate ceramics
CN106116567B (en) * 2016-06-22 2018-11-02 刘和来 The preparation method of high density nano barium titanate titanate ceramics
CN110078495A (en) * 2019-04-25 2019-08-02 北京元六鸿远电子科技股份有限公司 The adjustable wide temperature range medium ceramic material of dielectric constant
CN110078495B (en) * 2019-04-25 2022-05-10 北京元六鸿远电子科技股份有限公司 Dielectric constant adjustable wide temperature range medium ceramic material
CN110577401A (en) * 2019-08-14 2019-12-17 天津大学 preparation method of titanium dioxide-based dielectric material
CN113880573A (en) * 2021-09-10 2022-01-04 天津大学 Temperature-stable low-dielectric-loss microwave dielectric ceramic material and preparation method thereof
CN114853468A (en) * 2022-03-23 2022-08-05 哈尔滨理工大学 High-dielectric low-loss doped barium calcium titanate ceramic and preparation method thereof
CN114940616A (en) * 2022-04-08 2022-08-26 桂林理工大学 Rare earth modified strontium titanate giant dielectric ceramic material and preparation method thereof

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