CN103524127A - High-frequency grain boundary layer ceramic capacitor medium and preparation method - Google Patents
High-frequency grain boundary layer ceramic capacitor medium and preparation method Download PDFInfo
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Abstract
The invention relates to the technical field of inorganic non-metallic materials, and especially relates to a high-frequency grain boundary layer ceramic capacitor medium and a preparation method. The ingredients of the formula comprise, by weight, 88-96% of (Sr0.96Ba0.04)TiO3, 0.1-3% of Ba(Li1/4Nb3/4)O3, 0.1-4% of Dy2O3, 0.1-2.0% of SiO2, 0.1-2.5% of Al2O3, 0.03-2.0% of SrCO3, 0.1-2.0% of ZnO-Li2O-Bi2O3 glass powder (ZLB) and 0.01-2% of CuO. The high-frequency grain boundary layer ceramic capacitor medium without lead or cadmium is prepared and obtained through a conventional preparation method for a ceramic capacitor medium and a one-time sintering process method by utilization of common chemical raw materials of capacitor ceramics, and the sintering temperature of the capacitor ceramics can be lowered. The medium is suitable for preparation of single-sheet ceramic capacitors and single-layer sheet-type ceramic capacitors.
Description
Technical field
The present invention relates to technical field of inorganic nonmetallic materials, refer in particular to a kind of high frequency boundary ceramics condenser dielectric and preparation method thereof, it adopts conventional ceramic capacitor dielectric preparation method and once sintered processing method, utilize condenser ceramics general chemistry raw material, prepare unleaded, high frequency boundary ceramics condenser dielectric without cadmium, can also reduce the sintering temperature of condenser ceramics, this medium is suitable for preparing monolithic ceramic capacitor and individual layer chip ceramic capacitor, can greatly reduce the cost of ceramic condenser, this medium specific inductivity is higher, easily realize the miniaturization of ceramic condenser, and good temp characteristic, can improve proof voltage and dispersion frequency high to expand the range of application of boundary ceramics electrical condenser simultaneously, and free from environmental pollution in preparation and use procedure, safe.
Background technology
Along with developing rapidly with universal of surface mounting technique, the occupation rate of surface mount component (SMC) in electronics steadily improves, 1997, World Developed Countries electronic devices and components chip rate reached more than 70%, and the whole world is average more than 40%, and 2000, whole world electronic devices and components chip rate reached 70%, 2002 year, and chip rate surpasses 85%, in particular for adapting to the national defence leading-edge fields such as message area and aerospace to small-size multifunction electronics device urgent need day by day, portability, miniaturization and the multifunction trend of complying with command, control, communications, and information terminal, electronic element has entered the all-round developing new period, individual layer chip semiconductor ceramic material is divided into surperficial stratotype and crystal boundary stratotype two classes, is characterized in that volume is little, capacity is large, and in addition, intergranular semiconductor stupalith also has that good temp characteristic, frequency response characteristic are good, operating frequency advantages of higher, at present in the world, only have AVX, JOHANSON etc. can provide individual layer chip semiconductor ceramic material less than ten companies, the whole world to the market aggregate demand of individual layer chip semiconductor ceramic material element up to 4,500,000,000/year, for adapting to an urgent demand day by day of electronic devices and components microminiaturization, lightness, Composite, high frequency and high performance, semiconductor ceramic material is in miniaturization, high-k, high precision int and high frequency aspect are developed rapidly, and individual layer chip semiconductor ceramic material is the trend of development, the sintering temperature of general monolithic boundary ceramics condenser dielectric and individual layer chip boundary ceramics condenser dielectric is 1350 ~ 1430 ℃, there are the following problems simultaneously: otherwise withstand voltage lower, temperature factor is larger, specific inductivity is lower, sintering process is all to adopt double sintering method substantially, that is: first high temperature reduction, then applies insulation oxide and carry out oxidizing thermal treatment in middle temperature, technique is more complicated, and cost is higher, some adopts cladding process, and technique is more complicated, and raw material is more expensive, and cost is also higher, and boundary ceramics condenser dielectric sintering temperature of the present invention is 1270 ~ 1290 ℃ of left and right, adopt once sintered technique (first binder removal before 500 ℃ in nitrogen simultaneously, then after higher than 1000 ℃ with heat up at a slow speed (30 ~ 50 ℃/h), then in 3 ~ 5 hours sintering of 1270 ~ 1290 ℃ of insulations, then ℃ left and right, Slow cooling to 900 ~ 950 is incubated processing in 2 ~ 3 hours in air, last furnace cooling), can greatly reduce the cost of boundary ceramics electrical condenser like this, the not leaded and cadmium of this patent capacitor ceramic dielectric simultaneously, condenser ceramics is free from environmental pollution in preparation and use procedure, in addition, the specific inductivity of condenser ceramics of the present invention is high, can improve like this capacity and the miniaturization of ceramic condenser, meets the development trend of ceramic condenser, equally also can reduce the cost of ceramic condenser, boundary ceramics condenser dielectric proof voltage of the present invention is high, dispersion frequency is high, holds use range and security that requirement etc. that temperature characteristics meets X7R is conducive to expand boundary ceramics electrical condenser.
Summary of the invention
The object of this invention is to provide a kind of high frequency boundary ceramics condenser dielectric.
The object of the present invention is achieved like this:
High frequency boundary ceramics condenser dielectric formula forms and comprises (weight percent): (Sr
0.96ba
0.04) TiO
388-96%, Ba (Li
1/4nb
3/4) O
30.1-3%, Dy
2o
30.1-4%, SiO
20.1-2.0%, Al
2o
30.1-2.5%, SrCO
30.03-2.0%, ZnO-Li
2o-Bi
2o
3glass powder (ZLB) 0.1-2.0%, CuO0.01-2%; (Sr wherein
0.96ba
0.04) TiO
3, Ba (Li
1/4nb
3/4) O
3and ZnO-Li
2o-Bi
2o
3glass powder is respectively to adopt conventional chemical feedstocks synthetic with solid phase method.
(Sr used in medium of the present invention
0.96ba
0.04) TiO
3adopt following technique to prepare: by conventional chemical feedstocks SrCO
3and BaCO
3and TiO
2press 0.96:0.04:1 molar ratio ingredient, after ground and mixed is even, put into alumina crucible in 1250 ~ 1280 ℃ of insulations 120 minutes, solid state reaction is synthesized (Sr
0.96ba
0.04) TiO
3, ground 200 mesh sieves after cooling, standby.
Ba (Li used in medium of the present invention
1/4nb
3/4) O
3adopt following technique to prepare: by conventional chemical feedstocks BaCO
3and Li
2cO
3and Nb
2o
5press 1:1/8:3/8 molar ratio ingredient, after ground and mixed is even, put into alumina crucible in 700 ℃ of insulations 120 minutes, solid state reaction is synthesized Ba (Li
1/4nb
3/4) O
3, ground 200 mesh sieves after cooling, standby.
ZnO-Li used in medium of the present invention
2o-Bi
2o
3glass powder (ZLB) adopts following technique to prepare: by conventional chemical feedstocks ZnO and Li
2cO
3and Bi
2o
3press 1:0.5:0.5 molar ratio ingredient, ground and mixed is put into alumina crucible after evenly and is incubated 120 minutes in 600-650 ℃, and quenching in water then obtains ZnO-Li after cooling
2o-Bi
2o
3glass powder, ground 200 mesh sieves, standby.
The present invention adopts following high frequency boundary ceramics medium preparation technology: first adopt conventional chemical feedstocks to synthesize respectively (Sr with solid phase method
0.96ba
0.04) TiO
3, Ba (Li
1/4nb
3/4) O
3, ZnO-Li
2o-Bi
2o
3glass powder, then by formula batching, admixtion ball mill pulverizing is mixed, after drying, add tackiness agent granulation, be pressed into again green sheet, then in air, carry out binder removal and sintering (first binder removal before 500 ℃ in nitrogen, then after higher than 1000 ℃ with heat up at a slow speed (30 ~ 50 ℃/h), then in 3 ~ 5 hours sintering of 1270 ~ 1290 ℃ of insulations, then Slow cooling to 900 ~ 950 ℃ are incubated processing in 2 ~ 3 hours in air, last furnace cooling), obtain high frequency boundary ceramics condenser dielectric, on medium by electrode.
Described dielectric withstanding voltage is higher, and direct current proof voltage is 6.2-6.9kV/mm; Specific inductivity is high, is 30103-31515; Dispersion frequency (f
m) be 2.1-2.8GHz; Dielectric loss is 78-86 * 10
-4; Percentage of capacitance variation with temperature is little, meets the requirement of X7R characteristic; Insulation resistance is 70-85 * 10
10Ω cm.
The formula of above-mentioned ceramic dielectic preferably adopts following two kinds of schemes (weight percent):
(Sr
0.96ba
0.04) TiO
389-94%, Ba (Li
1/4nb
3/4) O
30.3-2.5%, Dy
2o
30.3-3.5%, SiO
20.1-1.5%, Al
2o
30.1-2%, SrCO
30.05-1.6%, ZnO-Li
2o-Bi
2o
3glass powder (ZLB) 0.2-1.8%, CuO0.06-2%;
(Sr
0.96ba
0.04) TiO
390-94%, Ba (Li
1/4nb
3/4) O
30.3-2.0%, Dy
2o
30.3-2.8%, SiO
20.1-1.3%, Al
2o
30.1-1.6%, SrCO
30.08-1.5%, ZnO-Li
2o-Bi
2o
3glass powder (ZLB) 0.3-1.5%, CuO0.1-1.8%.
Compared with prior art, tool has the following advantages in the present invention:
1, the medium of this patent adopts following once sintered technique: first binder removal before 500 ℃ in nitrogen, then after higher than 1000 ℃ with heat up at a slow speed (30 ~ 50 ℃/h), then in 3-5 hour sintering of 1270 ~ 1290 ℃ of insulations, then Slow cooling to 900 ~ 950 ℃ are incubated processing in 2 ~ 3 hours in air, last furnace cooling; Can greatly reduce the cost of ceramic condenser like this, not leaded and cadmium in the media components of this patent, environmentally safe.
2, the specific inductivity of this medium is high, is more than 30000; Proof voltage is high, more than direct current proof voltage can reach 6kV/mm; Dielectric loss is little, is less than 1.0%; Dispersion frequency (f
m) height, dispersion frequency (f
m) up to more than 2GHz; The specific inductivity of this medium is high, can realize miniaturization and the large capacity of ceramic condenser, can reduce costs equally.
3, the temperature factor of this medium is low, and percentage of capacitance variation with temperature is little, meets the requirement of X7R characteristic; Dielectric loss is less than 1.0%, and use procedure performance good stability is safe.
4, main raw material employing ceramic condenser level is pure can produce ceramic dielectic of the present invention.
5, this medium adopts conventional solid phase method ceramic capacitor dielectric preparation technology and a reduction-oxidation sintering process to be prepared.
Embodiment
The invention will be further described in conjunction with the embodiments now, and table 1 provides the embodiments of the invention formula of totally 4 samples.
The embodiments of the invention main raw material of the formula of totally 4 samples adopt the pure raw material of ceramic condenser level, first adopt in the preparation conventional chemical feedstocks to synthesize respectively (Sr with solid phase method
0.96ba
0.04) TiO
3, Ba (Li
1/4nb
3/4) O
3and ZnO-Li
2o-Bi
2o
3glass powder, then by above-mentioned formula batching, with distilled water or deionized water, adopt planetary ball mill ball milling to mix in the material preparing, material: ball: water=1:3:(0.6 ~ 1.0) (mass ratio), after ball milling 4 ~ 8 hours, dry to obtain dry mash, in dry mash, add and account for the polyvinyl alcohol solution that the concentration of its weight 8 ~ 10% is 10wt%, carry out granulation, mixed rear mistake 40 mesh sieves, under 20 ~ 30Mpa pressure, carry out again dry-pressing and become green sheet, first binder removal before 500 ℃ in nitrogen, then after higher than 1000 ℃ with heat up at a slow speed (30 ~ 50 ℃/h), then in 3 ~ 5 hours sintering of 1270 ~ 1290 ℃ of insulations, then be cooled to 900 ~ 950 ℃ in air, to be incubated processing in 2 ~ 3 hours, last furnace cooling, at 780 ~ 800 ℃, be incubated 15 minutes again and carry out silver ink firing, form silver electrode, solder taul again, seal, obtain boundary ceramics electrical condenser, test its dielectric properties.
Above-mentioned dielectric properties of respectively filling a prescription sample are listed in table 2, and prepared condenser ceramics proof voltage is higher as can be seen from Table 2, more than direct current proof voltage can reach 6kV/mm; Specific inductivity is high, is more than 30000; Dispersion frequency (f
m) up to more than 2GHz; Dielectric loss is less than 1.0 %; Percentage of capacitance variation with temperature is little, meets the requirement of X7R characteristic.
Table 1 embodiments of the invention are the formula of totally 4 samples
Respectively the fill a prescription dielectric properties of sample of table 2
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (7)
1. a high frequency boundary ceramics condenser dielectric, is characterized in that described medium composition according to weight percent calculating is: (Sr
0.96ba
0.04) TiO
388-96%, Ba (Li
1/4nb
3/4) O
30.1-3%, Dy
2o
30.1-4%, SiO
20.1-2.0%, Al
2o
30.1-2.5%, SrCO
30.03-2.0%, ZnO-Li
2o-Bi
2o
3glass powder 0.1-2.0%, CuO0.01-2%; (Sr wherein
0.96ba
0.04) TiO
3, Ba (Li
1/4nb
3/4) O
3and ZnO-Li
2o-Bi
2o
3glass powder is respectively to adopt conventional chemical feedstocks synthetic with solid phase method.
2. a kind of high frequency boundary ceramics condenser dielectric as claimed in claim 1, is characterized in that: described dielectric withstanding voltage is higher, and direct current proof voltage is 6.2-6.9kV/mm; Specific inductivity is high, is 30103-31515; Dispersion frequency (f
m) be 2.1-2.8GHz; Dielectric loss is 78-86 * 10
-4; Percentage of capacitance variation with temperature is little, meets the requirement of X7R characteristic; Insulation resistance is 70-85 * 10
10Ω cm.
3. a kind of high frequency boundary ceramics condenser dielectric as claimed in claim 1, is characterized in that: described (Sr
0.96ba
0.04) TiO
3adopt following technique to prepare: by conventional chemical feedstocks SrCO
3and BaCO
3and TiO
2press 0.96:0.04:1 molar ratio ingredient, after ground and mixed is even, put into alumina crucible in 1250 ~ 1280 ℃ of insulations 120 minutes, solid state reaction is synthesized (Sr
0.96ba
0.04) TiO
3, ground 200 mesh sieves after cooling, standby.
4. a kind of high frequency boundary ceramics condenser dielectric as claimed in claim 1, is characterized in that: described Ba (Li
1/4nb
3/4) O
3adopt following technique to prepare: by conventional chemical feedstocks BaCO
3and Li
2cO
3and Nb
2o
5press 1:1/8:3/8 molar ratio ingredient, after ground and mixed is even, put into alumina crucible in 700 ℃ of insulations 120 minutes, solid state reaction is synthesized Ba (Li
1/4nb
3/4) O
3, ground 200 mesh sieves after cooling, standby.
5. a kind of high frequency boundary ceramics condenser dielectric as claimed in claim 1, is characterized in that: described ZnO-Li
2o-Bi
2o
3glass powder adopts following technique to prepare: by conventional chemical feedstocks ZnO and Li
2cO
3and Bi
2o
3press 1:0.5:0.5 molar ratio ingredient, ground and mixed is put into alumina crucible after evenly and is incubated 120 minutes in 600-650 ℃, and quenching in water then obtains ZnO-Li after cooling
2o-Bi
2o
3glass powder, ground 200 mesh sieves, standby.
6. a kind of high frequency boundary ceramics condenser dielectric as claimed in claim 1, is characterized in that described medium composition according to weight percent calculating is: (Sr
0.96ba
0.04) TiO
389-94%, Ba (Li
1/4nb
3/4) O
30.3-2.5%, Dy
2o
30.3-3.5%, SiO
20.1-1.5%, Al
2o
30.1-2%, SrCO
30.05-1.6%, ZnO-Li
2o-Bi
2o
3glass powder 0.2-1.8%, CuO0.06-2%;
A kind of high frequency boundary ceramics condenser dielectric as claimed in claim 1, is characterized in that described medium composition according to weight percent calculating is: (Sr
0.96ba
0.04) TiO
390-94%, Ba (Li
1/4nb
3/4) O
30.3-2.0%, Dy
2o
30.3-2.8%, SiO
20.1-1.3%, Al
2o
30.1-1.6%, SrCO
30.08-1.5%, ZnO-Li
2o-Bi
2o
3glass powder 0.3-1.5%, CuO0.1-1.8%.
7. the preparation method of a kind of high frequency boundary ceramics condenser dielectric as claimed in claim 1, is characterized in that comprising the steps: to adopt conventional chemical feedstocks to synthesize respectively (Sr with solid phase method
0.96ba
0.04) TiO
3, Ba (Li
1/4nb
3/4) O
3and ZnO-Li
2o-Bi
2o
3glass powder, then by above-mentioned formula batching, with distilled water or deionized water, adopt planetary ball mill ball milling to mix in the material preparing, material: ball: water=1:3:(0.6 ~ 1.0) (mass ratio), after ball milling 4 ~ 8 hours, dry to obtain dry mash, in dry mash, add and account for the polyvinyl alcohol solution that the concentration of its weight 8 ~ 10% is 10wt%, carry out granulation, mixed rear mistake 40 mesh sieves, under 20 ~ 30Mpa pressure, carry out again dry-pressing and become green sheet, first binder removal before 500 ℃ in nitrogen, then the speed with 30 ~ 50 ℃/h heats up after higher than 1000 ℃, then in 3 ~ 5 hours sintering of 1270 ~ 1290 ℃ of insulations, then be cooled to 900 ~ 950 ℃ in air, to be incubated processing in 2 ~ 3 hours, last furnace cooling, at 780 ~ 800 ℃, be incubated 15 minutes again and carry out silver ink firing, form silver electrode, solder taul again, seal, obtain boundary ceramics electrical condenser.
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|---|---|---|---|
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|---|---|---|---|
| CN201310462413.7A CN103524127B (en) | 2013-10-08 | 2013-10-08 | High-frequency grain boundary layer ceramic capacitor medium and preparation method |
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|---|---|
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| CN103524127B CN103524127B (en) | 2015-03-04 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105272362A (en) * | 2015-11-10 | 2016-01-27 | 电子科技大学 | Grain boundary layer semiconductor ceramic chip oxidizer coating material and preparation method thereof |
| CN106587996A (en) * | 2016-11-14 | 2017-04-26 | 江苏大学 | High-frequency granular-boundary-layer ceramic capacitor dielectric |
| CN106587989A (en) * | 2016-11-15 | 2017-04-26 | 江苏大学 | High-dielectric performance grain boundary layer ceramic capacitor medium |
| CN106631005A (en) * | 2017-01-10 | 2017-05-10 | 北京元六鸿远电子科技股份有限公司 | Lead-free high-voltage capacitor dielectric ceramic sintered at medium temperature and preparation method thereof |
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| US4379854A (en) * | 1981-02-06 | 1983-04-12 | Erie Technological Products, Inc. | Low temperature firing (1800°-2100° F.) of barium titanate with flux (lead titanate-bismuth titanate-zinc oxide and boron oxide) |
| US4642732A (en) * | 1985-04-26 | 1987-02-10 | Tdk Corporation | Dielectric ceramic composition and method of producing same, and a monolithic capacitor |
| CN102436929A (en) * | 2011-07-22 | 2012-05-02 | 中国科学院上海硅酸盐研究所 | High-dielectric low-loss imitation grain boundary layer capacitor and preparation method thereof |
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2013
- 2013-10-08 CN CN201310462413.7A patent/CN103524127B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US4379854A (en) * | 1981-02-06 | 1983-04-12 | Erie Technological Products, Inc. | Low temperature firing (1800°-2100° F.) of barium titanate with flux (lead titanate-bismuth titanate-zinc oxide and boron oxide) |
| US4642732A (en) * | 1985-04-26 | 1987-02-10 | Tdk Corporation | Dielectric ceramic composition and method of producing same, and a monolithic capacitor |
| CN102436929A (en) * | 2011-07-22 | 2012-05-02 | 中国科学院上海硅酸盐研究所 | High-dielectric low-loss imitation grain boundary layer capacitor and preparation method thereof |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105272362A (en) * | 2015-11-10 | 2016-01-27 | 电子科技大学 | Grain boundary layer semiconductor ceramic chip oxidizer coating material and preparation method thereof |
| CN105272362B (en) * | 2015-11-10 | 2017-06-30 | 电子科技大学 | Intergranular semiconductor potsherd oxidant coating material and preparation method thereof |
| CN106587996A (en) * | 2016-11-14 | 2017-04-26 | 江苏大学 | High-frequency granular-boundary-layer ceramic capacitor dielectric |
| CN106587996B (en) * | 2016-11-14 | 2020-03-31 | 江苏大学 | High-frequency grain boundary layer ceramic capacitor medium |
| CN106587989A (en) * | 2016-11-15 | 2017-04-26 | 江苏大学 | High-dielectric performance grain boundary layer ceramic capacitor medium |
| CN106587989B (en) * | 2016-11-15 | 2019-08-02 | 江苏大学 | A kind of high dielectric property grain boundary layer ceramic capacitor medium |
| CN106631005A (en) * | 2017-01-10 | 2017-05-10 | 北京元六鸿远电子科技股份有限公司 | Lead-free high-voltage capacitor dielectric ceramic sintered at medium temperature and preparation method thereof |
| CN106631005B (en) * | 2017-01-10 | 2020-01-14 | 北京元六鸿远电子科技股份有限公司 | Medium-temperature sintered lead-free high-voltage capacitor dielectric ceramic material and preparation method thereof |
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| CN103524127B (en) | 2015-03-04 |
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