CN1719559A - Barium titanate ceramic capacitor medium and preparing method thereof - Google Patents
Barium titanate ceramic capacitor medium and preparing method thereof Download PDFInfo
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- CN1719559A CN1719559A CN 200510014547 CN200510014547A CN1719559A CN 1719559 A CN1719559 A CN 1719559A CN 200510014547 CN200510014547 CN 200510014547 CN 200510014547 A CN200510014547 A CN 200510014547A CN 1719559 A CN1719559 A CN 1719559A
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Abstract
This invention discloses a condenser medium of barium titanate ceramics and its preparation method, which takes BaTiO3 as the main composition, its weight is 1 added by the following weight percentages: Nb2O5: 1.00~1.50%, CoCO3 0.1~0.5%, CeO2: 0.1~0.5% and a fusing agent: 0.25~0.50%. They are mixed to an adjuvant to be ball-ground, prilled and dry-pressed to a round green compact sheet to be burnt in oven under 1240deg.C to be insulated for 4-8 hours and cooled for 10 hours in the oven to be manufactured to a ceramic condenser medium. Since the dielectric constant of the medium is high the medium loss is small and its volume temperature absolute value is less than 13%, thermal stability is good, it can be used in producing large volume condensers or other electronic devices.
Description
Technical field
The present invention relates to a kind of dielectric ceramic compositions and preparation method, specifically, is a kind of barium titanate based ceramic medium and preparation method thereof.
Background technology
Along with the development of surface mounting technology in the electronic circuit, require the volume of multilayer ceramic capacitor (MLC) microminiaturized more, this just needs, and capacitance is bigger, the better dielectric material of thermal stability.Be used to make the main at present X7R of the employing type of the dielectric material ceramic material of low-frequency high dielectric thermostable type MLC, what X7R represented is a kind of appearance temperature characteristics, promptly in-55～+ 125 ℃ of scopes, and its capacity rate of temperature change | Δ C/C
25 ℃|≤15%.Such capacitor is widely used in the coupling circuit of high-grade electronic equipment such as mobile phone, and in its forward and backward level transmission course, the distortion of signal should be as much as possible little, and this will depend on the capacity of coupling capacitance and hold temperature characteristics.Kind as X7R ceramic capacitor dielectric material is a lot, the more common ceramic material that the ferroelectric series ceramic material of lead base relaxation, tungsten bronze ore deposit structure are arranged, barium phthalate base ferroelectric ceramic material etc., because the ferroelectric series ceramic material of lead base contains a large amount of lead, can cause very big harm to human body and environment, preparation process condition must strictly be controlled; The series ceramic material loss of tungsten bronze ore deposit is big and dielectric property are unstable, therefore, is that basic dielectric ceramic is the emphasis that people pay close attention to always with the barium titanate.Chinese patent 98124799.7 discloses a kind of composition and preparation method of temperature-stable high dielectric multi-layer ceramic capacitor material, and this material is based on barium titanate, and additive is Co
2O
3, Nb
2O
5, rare earth oxide and MnO
2, its room temperature dielectric constant can reach 4400, temperature coefficient of capacitance≤± 15%, and resistivity is 10
12～13Ω cm, though the performance of this ceramic material can satisfy the instructions for use of X7R capacitor, its dielectric constant is not enough big, and dielectric loss is not mentioned, two step process of sintering again after its preparation method still adopts raw material synthetic in addition are so cost of manufacture is higher.
Summary of the invention
Technical problem to be solved by this invention provides a kind of dielectric loss tan δ≤0.016, and dielectric constant bigger (＞4400), height Jie thermostable type ceramic capacitor dielectric of temperature coefficient of capacitance≤± 13% improves preparation technology simultaneously, reduces cost of manufacture.
For realizing above-mentioned task, the technical solution used in the present invention is: designed a kind of barium titanate ceramic capacitor medium, this medium is with BaTiO
3Being principal component, is 1 by its weight, adds the composition of following weight percentage and forms: 1.00～1.50% Nb
2O
5, 0.10～0.50% CoCO
3, 0.10～0.50% CeO
2, 0.25～0.50% glass.In above-mentioned composition, described BaTiO
3Be the pure BaTiO of analysis of calcining
3Described glass is by Bi
2O
3, B
2O
3, SiO
2Formed by weight 40: 8: 8.
The present invention also provides a kind of preparation method of above-mentioned barium titanate ceramic capacitor medium, and it follows these steps to carry out:
(1) at first will analyze pure BaTiO
3Calcining is heated to 1160～1200 ℃ by the heating rate of 6～7 ℃/min, be incubated 2 hours, cools off afterwards standby;
(2) with Bi
2O
3, B
2O
3, SiO
2Mixed by weight 40: 8: 8, melt quenching promptly makes glass;
(3) by calcining BaTiO
3Weight be 1, add the Nb of percetage by weight 1.00～1.50%
2O
5, 0.10～0.50% CoCO
3, 0.10～0.50% CeO
2, 0.25～0.50% preparing glass charge, added the deionized water ball milling 8 hours with zirconia ball, cross 250 holes/em in 120 ℃ of dry backs
2Sub-sieve, the paraffin granulation that adds 6～7wt% then, under 60～80MPa pressure, be pressed into the disk green compact, putting into electric furnace at last burns till, heating rate by 3 ℃/min is heated to 500 ℃ earlier, heating rate by 6 ℃/min is heated to 1240 ℃ again, is incubated 4～8 hours, promptly makes ceramic dielectric in 10 hours with the stove cooling.
BaTiO in the above-mentioned steps (1)
3Calcining heat be preferably 1180～1200 ℃; The temperature retention time of burning till of disk green compact is preferably 6～8 hours in the step (3).
Has very high dielectric constant (the highest by 4811) by the prepared ceramic dielectric of the present invention, and has good thermal stability (the capacity rate of temperature change is in ± 13%), on the other hand, cost of material of the present invention is cheap, preparation section is simplified, and promptly the batching back only needs a ball milling, and cost of manufacture is lower, can be used as the replacement product of same type of material, good market prospects are arranged.Beneficial effect of the present invention also will further be set forth in following embodiment.
Embodiment
Example 1:
(1) at first with analytically pure BaTiO
3Calcining is heated to 1160～1200 ℃ by the heating rate of 6～7 ℃/min, be incubated 2 hours, cools off afterwards standby;
(2) with Bi
2O
3, B
2O
3, SiO
2Mixed by weight 40: 8: 8, melt quenching promptly makes glass;
(3) by calcining BaTiO
3Weight be 100g, add 1.25g Nb
2O
5, 0.35g CoCO
3, 0.5gCeO
2, the 0.25g preparing glass charge, it forms code name is A, adds the deionized water ball milling 8 hours with zirconia ball, crosses 250 holes/cm with electrically heated drying cabinet after 120 ℃ of oven dry
2Sub-sieve, the paraffin granulation that adds 6～7wt% then, being pressed into diameter under 60～80MPa pressure is 15mm, thickness is the disk green compact of 2mm, put it in the electric furnace at last and burn till, the heating rate by 3 ℃/min is heated to 500 ℃ earlier, and the heating rate by 6 ℃/min is heated to 1240 ℃ again, be incubated 4～8 hours, promptly made ceramic dielectric in 10 hours with the stove cooling.
The ceramic dielectric that sinters reburned ooze silver electrode, welding lead is made the capacitor sample; Under 1MHz, survey its capacitance C and loss tangent tan δ with HewlettPackard4278A Capacitance Meter, and the relative dielectric constant ε of calculation medium; Measure its capacity rate of temperature change with GZ-ESPEC insulating box and HM27002 type capacitor C-T characteristic tester.
Example 2:
By calcining BaTiO
3Weight be 100g, add 1.00g Nb
2O
5, 0.50g CoCO
3, 0.25g CeO
2, the 0.50g preparing glass charge, it forms code name is B, the preparation of all the other process conditions and capacitor sample and measurement are with example 1.
Example 3:
By calcining BaTiO
3Weight be 100g, add 1.50gNb
2O
5, 0.10g CoCO
3, 0.10g CeO
2, the 0.35g preparing glass charge, it forms code name is C, the preparation of all the other process conditions and capacitor sample and measurement are with example 1.
Form among the embodiment above-mentioned three of the present invention, need benly be the BaTiO of its step (1)
3Divide three temperature spots: 1160 ℃, 1180 ℃ and 1200 ℃ of calcinings; The temperature retention time of burning till in the step (3) is divided into three periods: carried out in 4 hours, 6 hours and 8 hours; Each prescription is formed the BaTiO that all calcines with above-mentioned three different temperature points
3Batching obtains three groups of dry-pressing green compact respectively, will form then among A～C with 1160 ℃ of calcining BaTiO
3It is one group that the dry-pressing green compact of batching are respectively got three, burns till at 1240 ℃ simultaneously, is incubated 4～8 hours; To form among A～C with 1180 ℃ of calcining BaTiO
3It is one group that the dry-pressing green compact of batching are respectively got three, burns till at 1240 ℃ simultaneously, is incubated 4～8 hours; To form among A～C with 1200 ℃ of calcining BaTiO
3It is one group that the dry-pressing green compact of batching are respectively got three, burns till at 1240 ℃ simultaneously, is incubated 4～8 hours; Make 27 capacitor samples at last, survey its dielectric property, test result is listed in the table 1.
By the test result of table 1 as can be seen, three compositions of ceramic dielectric of the present invention burn till at 1240 ℃, and its dielectric constant is with the increase (4～8 hours) and the BaTiO of temperature retention time
3The rising of calcining heat (1160 ℃～1200 ℃) and increasing considerably, though and dielectric loss increases to some extent with holding time prolonging, but change little, all in 0.016; Temperature coefficient of capacitance has increase tendency with holding time prolonging, but in the present invention, all be controlled at ± 13% in; In addition, the CeO during the loss of the present invention's composition and temperature coefficient of capacitance are formed with porcelain
2The increase of content and slightly giving adds, but all in the instructions for use scope of X7R, but CeO
2Effect bigger to the contribution of dielectric constant, this can find out from the listed data of table 1.Therefore, as can be known, the present invention preferably consists of A from the data of table 1, and preferred process conditions are: a) prepare burden with the BaTiO of 1180～1200 calcinings
3For good; The temperature retention time of b) burning till be 6～8 hours for well, its ε of prepared ceramic dielectric is more than 4400, maximum can reach 4811.
Barium titanate ceramic capacitor medium of the present invention is owing to its dielectric constant height (4400～4800), dielectric loss are little, the absolute value of tan δ≤0.016, capacity rate of temperature change≤13%, therefore Heat stability is good can be used for making the electronic device of big capacity, temperature-stable coupling capacitor or similar applications in the high-grade electronic equipment.
Dielectric property under the table 1 barium titanate ceramic capacitor medium sample of the present invention different technology conditions
| Form code name | BaTiO 3Calcining heat ℃ (being incubated 2 hours) | 1240 ℃ burn till temperature retention time (hour) | The sample dielectric property | ||
| ε | tanδ | Max |ΔC/C 25□|(％) | |||
| A | 1160 | 8 | 4580 | 0.015 | 11.72 |
| 6 | 4335 | 0.014 | 9.63 | ||
| 4 | 4229 | 0.013 | 8.82 | ||
| 1180 | 8 | 4724 | 0.016 | 11.78 | |
| 6 | 4428 | 0.016 | 10.93 | ||
| 4 | 4270 | 0.014 | 10.02 | ||
| 1200 | 8 | 4811 | 0.015 | 12.12 | |
| 6 | 4651 | 0.014 | 11.29 | ||
| 4 | 4446 | 0.014 | 9.63 | ||
| B | 1160 | 8 | 4460 | 0.014 | 10.38 |
| 6 | 4258 | 0.013 | 8.49 | ||
| 4 | 4115 | 0.013 | 7.35 | ||
| 1180 | 8 | 4562 | 0.015 | 10.86 | |
| 6 | 4337 | 0.014 | 9.18 | ||
| 4 | 4205 | 0.013 | 8.23 | ||
| 1200 | 8 | 4650 | 0.016 | 11.52 | |
| 6 | 4443 | 0.015 | 9.52 | ||
| 4 | 4299 | 0.014 | 7.87 | ||
| C | 1160 | 8 | 4309 | 0.015 | 9.15 |
| 6 | 4158 | 0.014 | 7.75 | ||
| 4 | 4007 | 0.013 | 6.33 | ||
| 1180 | 8 | 4469 | 0.015 | 9.83 | |
| 6 | 4312 | 0.015 | 8.51 | ||
| 4 | 4168 | 0.013 | 7.25 | ||
| 1200 | 8 | 4623 | 0.015 | 10.03 | |
| 6 | 4422 | 0.014 | 8.73 | ||
| 4 | 4279 | 0.014 | 6.99 | ||
Claims (6)
1. a barium titanate ceramic capacitor medium is characterized in that it is with BaTiO
3Being principal component, is 1 by its weight, adds the composition of following weight percentage and forms: 1.00～1.50% Nb
2O
5, 0.10～0.50% CoCO
3, 0.10～0.50% CeO
2, 0.25～0.50% glass.
2. barium titanate ceramic capacitor medium according to claim 1 is characterized in that, described BaTiO
3Be the BaTiO of calcining
3
3. barium titanate ceramic capacitor medium according to claim 1 and 2 is characterized in that described glass is by Bi
2O
3, B
2O
3, SiO
2Formed by weight 40: 8: 8.
4. the preparation method of a barium titanate ceramic capacitor medium is characterized in that, it follows these steps to carry out:
(1) at first with BaTiO
3Calcining is heated to 1160～1200 ℃ by the heating rate of 6～7 ℃/min, be incubated 2 hours, cools off afterwards standby;
(2) with Bi
2O
3, B
2O
3, SiO
2Mixed by weight 40: 8: 8, melt quenching promptly makes glass;
(3) by calcining BaTiO
3Weight be 1, add the Nb of percetage by weight 1.00～1.50%
2O
5, 0.10～0.50% CoCO
3, 0.10～0.50% CeO
2, 0.25～0.50% preparing glass charge, added the deionized water ball milling 8 hours with zirconia ball, cross 250 holes/cm in 120 ℃ of dry backs
2Sub-sieve, the paraffin granulation that adds 6～7wt% then, under 60～80MPa pressure, be pressed into the disk green compact, putting into electric furnace at last burns till, heating rate by 3 ℃/min is heated to 500 ℃ earlier, heating rate by 6 ℃/min is heated to 1240 ℃ again, is incubated 4～8 hours, promptly makes ceramic dielectric in 10 hours with the stove cooling.
5. the preparation method of barium titanate ceramic capacitor medium according to claim 4 is characterized in that, BaTiO in the described step (1)
3Calcining heat be 1180～1200 ℃.
6. the preparation method of barium titanate ceramic capacitor medium according to claim 4 is characterized in that, the temperature retention time that the disk green compact burn till in the described step (3) is 6～8 hours.
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| CNB2005100145478A CN100452257C (en) | 2005-07-15 | 2005-07-15 | Barium titanate ceramic capacitor medium and preparing method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100145478A CN100452257C (en) | 2005-07-15 | 2005-07-15 | Barium titanate ceramic capacitor medium and preparing method thereof |
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|---|---|
| CN1719559A true CN1719559A (en) | 2006-01-11 |
| CN100452257C CN100452257C (en) | 2009-01-14 |
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|---|---|---|---|
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100415682C (en) * | 2006-12-27 | 2008-09-03 | 天津大学 | Temperature stable type barium titanate system ceramic and its preparation method |
| CN101033132B (en) * | 2007-02-13 | 2010-10-13 | 电子科技大学 | Middle-temperature sintering high temperature stabilization type ceramic capacitor dielectric material |
| CN101030478B (en) * | 2007-03-27 | 2010-11-17 | 天津大学 | High-dielectric metal-electric medium composite ceramic capacitance and its production |
| CN101698598B (en) * | 2009-11-06 | 2012-01-11 | 河北理工大学 | Dielectric ceramic suitable for working at rugged surrounding temperature and preparation method thereof |
| CN104725036A (en) * | 2015-02-10 | 2015-06-24 | 景德镇陶瓷学院 | High-temperature low-loss barium strontium titanate-based energy-storage ceramic and preparation method thereof |
| CN105801111A (en) * | 2016-04-20 | 2016-07-27 | 宝鸡雍鑫电子有限公司 | High-dielectric-constant ceramic capacitor ceramic material and preparing method thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61275164A (en) * | 1985-05-03 | 1986-12-05 | タム セラミツクス インコ−ポレイテツド | Dielectric ceramic composition having high permittivity and flat tc properties |
| CN1545112A (en) * | 2003-11-17 | 2004-11-10 | 天津大学 | Ceramic material of high-frequency ceramic capacitor and method for manufacturing same |
| CN100364924C (en) * | 2003-12-29 | 2008-01-30 | 广东风华高新科技集团有限公司 | Titanium barium base ceramic medium materials and capacitor made thereform |
-
2005
- 2005-07-15 CN CNB2005100145478A patent/CN100452257C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100415682C (en) * | 2006-12-27 | 2008-09-03 | 天津大学 | Temperature stable type barium titanate system ceramic and its preparation method |
| CN101033132B (en) * | 2007-02-13 | 2010-10-13 | 电子科技大学 | Middle-temperature sintering high temperature stabilization type ceramic capacitor dielectric material |
| CN101030478B (en) * | 2007-03-27 | 2010-11-17 | 天津大学 | High-dielectric metal-electric medium composite ceramic capacitance and its production |
| CN101698598B (en) * | 2009-11-06 | 2012-01-11 | 河北理工大学 | Dielectric ceramic suitable for working at rugged surrounding temperature and preparation method thereof |
| CN104725036A (en) * | 2015-02-10 | 2015-06-24 | 景德镇陶瓷学院 | High-temperature low-loss barium strontium titanate-based energy-storage ceramic and preparation method thereof |
| CN105801111A (en) * | 2016-04-20 | 2016-07-27 | 宝鸡雍鑫电子有限公司 | High-dielectric-constant ceramic capacitor ceramic material and preparing method thereof |
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|---|---|
| CN100452257C (en) | 2009-01-14 |
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