CN102336569A - Preparation method of ultralow-loss microwave dielectric ceramics and application of ultralow-loss microwave dielectric ceramics in radio-frequency/microwave capacitors - Google Patents
Preparation method of ultralow-loss microwave dielectric ceramics and application of ultralow-loss microwave dielectric ceramics in radio-frequency/microwave capacitors Download PDFInfo
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- CN102336569A CN102336569A CN2010102389001A CN201010238900A CN102336569A CN 102336569 A CN102336569 A CN 102336569A CN 2010102389001 A CN2010102389001 A CN 2010102389001A CN 201010238900 A CN201010238900 A CN 201010238900A CN 102336569 A CN102336569 A CN 102336569A
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Abstract
The invention discloses a preparation method of ultralow-loss microwave dielectric ceramics and application of ultralow-loss microwave dielectric ceramics in radio-frequency/microwave capacitors, and particularly relates to the technical field of manufacture of microwave dielectric ceramics. The principal component of the microwave dielectric ceramics is compounded from oxides of Nd, Ba and Ti as substrates, and at least one trace rare-earth oxide is added to the composition. A stirring and grinding production technique is introduced into the manufacturing technique of microwave dielectric ceramics, so that the repetitiveness and stability of the mass production technique of the microwave dielectric ceramics can be effectively controlled. When the microwave dielectric ceramics are used for manufacturing radio-frequency/microwave multi-layer ceramic capacitors, a dielectric ceramic diaphragm running processing technology and a multi-layer ceramic capacitor printing lamination production technology are utilized. The ultralow-loss microwave dielectric ceramics are sintered at moderate temperature; and the measurement on the product indicates that the dielectric constant is 52-54, the temperature coefficient is 0 (0+/-30 PPM/DEG C), loss is ultralow (0.0001-0.00002), and the Q value is high (>=10000-500000). The ultralow-loss microwave dielectric ceramics are a key material for manufacturing high-end electronic components of radio-frequency/microwave multi-layer ceramic capacitors.
Description
Technical field
The invention discloses the applied technical field that belongs in ultra-low loss microwave dielectric ceramic materials manufacturing technology field and the RF electrical condenser; Be particularly related to the Nd-Ba-Ti oxide compound and be the basis, formulated ultra-low loss microwave-medium ceramics preparation method and the application of RF laminated ceramic capacitor such as interpolation proper amount of rare-earth oxide compound.
Background technology
Laminated ceramic capacitor is one of maximum, with fastest developing speed electronic component of present consumption in the world.Laminated ceramic capacitor (MLCC) is mainly used in the concussion, coupling, filtering, bypass circuit of all kinds of military, civilian complete machines, and Application Areas has been extended to industries such as instrument for automatic control, computingmachine, mobile phone, digital household appliances, automobile electricity.At present, laminated ceramic capacitor has constituted the main body in electrical condenser market, the demand annual growth rate nearly 15% of world market.The market requirement is huge, and the industrialization market outlook are boundless.
The RF laminated ceramic capacitor has high withstand voltage, big electric current, high-power, ultrahigh Q-value, ultra-low equivalent series resistance ESR.The radio frequency power laminated ceramic capacitor is a present important developing direction.Though MgTiO
3, Ti9Ba
2O
2O, BaTi
4O
9With ceramics as low-loss microwave medium such as Nd-Ba-Ti; Carried out extensive studies and application by people already; But satisfy high-end electronic component (RF laminated ceramic capacitor) development and demand; Also there are sintering temperature high (1300 ℃～1350 ℃), Q value:＜10000 shortcoming, therefore use and receive very big restriction.Therefore, to researching and proposing of ultra-low loss microwave dielectric ceramic materials urgent requirement.
Summary of the invention
The object of the invention aims to provide a kind of specific inductivity 45～56, hi-q (Q value>=10000～500000), zero-temperature coefficient (0 ± 30PPM/ ℃), high insulation resistance>=10
12Ω, high dielectric withstanding voltage>=1800VDC/mil.Ultra-low loss microwave dielectric ceramic materials preparation method and the application in the RF laminated ceramic capacitor is produced.
For reaching above-mentioned performance index, the present invention adopts following media ceramic fabricating technology scheme to be achieved:
Ultra-low loss microwave dielectric ceramic materials preparation method, it is that it is 1 by synthetic weight of burning piece with the synthetic in advance piece that burns of Nd, Ba, Ti oxide compound staple, interpolation proper amount of rare-earth oxide compounds etc. are formulated.
Technology of preparing scheme of the present invention: like the described synthetic in advance piece that burns of, claim 1, the preparation method, by the Nd of the oxide components of following weight percentage ratio: 50～62wt%
2O
3, 7.1～15wt% BaCO
3, 35～45wt% TiO
2Form.Adopting purity is the oxide compound more than 99.6%; Synthesize the preparation method who burns piece by above-mentioned weight percentage weighing, mixing in advance through sintering; With the weighing by weight percentage of above-mentioned oxide compound; Ratio in powder 1, deionized water 0.8～1.2 adopts the stirring mill to mix 1～3 hour; Carry out granulation after drying 60 mesh sieves in 120 ± 5 ℃, pre-burning made above-mentioned powder reach preshrinking in 2～3 hours in 1160～1200 ℃ of sintering ovens that contain air atmosphere, and is compound and form loose dough and be commonly called as (synthetic in advance) and burn piece.
Technology of preparing scheme of the present invention: said ultra-low loss microwave dielectric ceramic materials and manufacturing side thereof are sent out, and prepare by following step:
Material formula makeup: it burns piece weight by synthetic in advance is 1, adds the composition of following weight percentage ratio: the Dy of 0.1～5wt%
2O
3, the Nb of 0.1～3.0wt%
2O
5, the Ta of 0.02～1.5wt%
2O
5, the ZrO of 0.05～2.5wt%
2, the Sm of 0.02～1.5wt%
2O
3, the wilkinite of 0.1～5wt%, the MnCO of 0.1～5wt%
3The above-mentioned at least two or more additives of interpolation etc. are formulated
The medium ceramic material preparation: said ultra-low loss microwave-medium ceramics preparation method is characterised in that adopt and stir the mill production technique, its technology controlling and process key element comprises following content.
(1) the grinding media material be the zirconia ball diameter (1～4mm), carry out stirring in 1～4 hour mill in ball-milling medium material 4, powder 1, deionized water 0.8～1.5 ratio.Discharging, subsequent use through 110～120 ℃ of oven dry, mistake 100 mesh sieves.
(2) test disk preparation: take by weighing the above-mentioned media ceramic material of 40～60 grams and add 2～6% heating paraffin mix, cool off, sieve (granulation), 100MPa compression molding, process microwave-medium ceramics trial circle chip capacitor device green compact.
(3) said test disk sintering: being characterised in that, is that the temperature rise rate with 3～6 ℃/min rose to 1130～1200 ℃ again after temperature rise rate with 1～2 ℃/min rose to 400 ℃.Be incubated 1.5～4 hours.Naturally cool to room temperature then.
The beneficial effect that the present invention obtained is that the multiple rare earth oxide of configuration of interpolation and science in the Nd-Ba-Ti basic system is in the synergy of sintering process owing to them; Reach the inhibition grain growth; Improve pottery and organize textural defect, obtain ultralow dielectric loss, high dielectric withstanding voltage; The media ceramic of high insulation resistance and zero-temperature coefficient has been obtained the double goal of ultra-low loss microwave-medium ceramics preparation method and the application in the RF electrical condenser.
Embodiment
Below in conjunction with specific embodiment technical scheme of the present invention is further specified.
The present invention adopts the Nd of 50～62wt%
2O
3, 7.1～15wt% BaCO
3, 35～45wt% TiO
2(purity is no less than 99.6%) is the initial oxidation raw material, adopts the synthetic in advance preparation method who burns piece, and utilizing the burning block of material is main moity, adds the Dy of following weight percentage composite: 0.1～5wt% again
2O
3, the Nb of 0.1～3.0wt%
2O
5, the Ta of 0.02～1.5wt%
2O
5, the ZrO of 0.05～2.5wt%
2, the Sm of 0.02～1.5wt%
2O
3, the wilkinite of 0.1～5wt%, the MnCO of 0.1～5wt%
3At least two or more additives launches the sample of medium ceramic material is made and electrical property research.
Embodiment 1: synthetic (Nd-Ba-Ti) pottery burns piece in advance, prepares according to the weighing of table one prescription.Concrete preparation method comprises the steps:
(1) with purity greater than the oxide compound more than 99.6, by the composition weighing of following weight percentage: the Nd of 50～62wt%
2O
3, 7.1～15wt% BaCO
3, 35～45wt% TiO
2Component.Adopt and stir mill mixing production technique; Above-mentioned oxide aggregate powder inserted in the agitator mill bucket stir the mill abrasive material in powder than the ratio of deionized water (1: 0.8～1.2) and mix, after mixing time is 1～3 hour, with 80 eye mesh screens filtration discharging; In 110～120 ℃ of oven dry; Pulverized and add 8～10% deionized water behind 40 eye mesh screens and carry out granulation, and pending presintering is synthetic in the saggar of packing into, burns piece and uses as the batching staple.
(2) the synthetic piece that burns of presintering rises to 1120～1160 ℃ with the temperature rise rate of 5～10 ℃/min.Being incubated 3 hours and naturally cooling to room temperature takes out subsequent use.
Embodiment 2: said medium ceramic material preparation method is characterised in that by above-mentioned synthetic in advance, burning piece weight is 1, adds the following weight percentage composite: the Dy of rare-earth oxidation raw material 0.1～5wt%
2O
3, the Nb of 0.1～3.0wt%
2O
5, the Ta of 0.02～1.5wt%
2O
5, the ZrO of 0.05～2.5wt%
2, the Sm of 0.02～1.5wt%
2O
3, the wilkinite of 0.1～5wt%, the MnCO of 0.1～5wt%
3At least add two or more rare earth oxides and constitute the media ceramic composition.Carry out weighing according to table 1 prescription.
Each oxide raw material weight unit of table 1 is gram
(1) takes by weighing oxide raw material respectively by table 1 prescription; Adopt and stir the mill producing process; The ratio of in the agitator mill bucket, inserting above-mentioned oxide compound and deionized water (1: 0.8～1.2) stirs after time consuming is 1～3 hour; Filter discharging with 80 eye mesh screens,, pulverized 100 eye mesh screens in 110～120 ℃ of oven dry;
Embodiment 3 media ceramics use the preparation of wafer capacitance device:
(1) takes by weighing the media ceramic powder of embodiment 2; Add 8.0～10.0wt% heating paraffin melt-blended, sieve, cooling, compression molding 100MPa, media ceramic wafer capacitance device sintering; Temperature rise rate with 8～10 ℃/min rises to 400 ℃; Temperature rise rate with 4～6 ℃/min rises to 1160～1200 ℃ (each of embodiment batch sintering temperature and soaking time are seen table 2) again, is cooled to room temperature then;
(2) preparation of media ceramic wafer capacitance device end electrode and silver ink firing: in the electrode coated slurry oven dry of media ceramic wafer capacitance device both ends of the surface, in 830～860 ℃ sintering temperature, carry out the silver electrode sintering, soaking time is taken out after being not less than the 30min naturally cooling;
(3) measurement of media ceramic wafer capacitance device electrical capacity and loss: use HP4278A or 4284A electrical capacity to measure the electrical capacity C of appearance, according to following calculation formula (1) calculation medium ceramic dielectric constant at 1MHZ frequency measurement wafer sample.
Formula (1)
ε＝14.4×C×d/D
2
Wherein: C is the electrical capacity of wafer sample, and unit is Pf; D is a thickness of sample, and unit is cm; D is the diameter of sample, and unit is cm.
(4) media ceramic wafer capacitance device insulation measurement: use HM2681 insulation measurement appearance to measure measuring voltage 500V, insulation resistance>=10
6M Ω.
(5) media ceramic wafer capacitance device dielectric withstanding voltage is measured: use AC/DC proof voltage survey meter to measure;
(6) media ceramic wafer capacitance actuator temperature coefficient is measured: use HP4278A electrical capacity measurement appearance and the high-low temperature chamber joint survey rate of change of capacitance at 1MHZ frequency measurement wafer sample, again the accounting temperature coefficient.
Medium ceramic material specific embodiment wafer capacitance device performance measurement result of the present invention sees table 2.
The performance measurement result of table 2 media ceramic wafer capacitance device
Embodiment 4 has described and has adopted ultra-low loss microwave dielectric ceramic materials of the present invention to make the manufacturing process and the product measurement performance of RF laminated ceramic capacitor product.
The dielectric ceramic diaphragm casting technique; Use the ultra-low loss microwave dielectric ceramic materials to carry out dielectric ceramic diaphragm curtain coating processing (curtain coating quantity 5KG; Medium diaphragm thickness 37); The medium diaphragm is as RF laminated ceramic capacitor key structure material, and the medium diaphragm is to realize basis multi-sheet printed, lamination.The dielectric ceramic powder body characteristics
(1) D50=0.669, powder density 5.43;
(2) printing of RF electrode multilayered ceramic capacitors slurry adopts handpress to carry out interior electrode printing lamination, and electrode size is a 30pd/70Ag printing slurry; Having made physical dimension respectively is: C type three end filters of 1.4 * 1.4mm, 2.8 * 2.8mm, 10.0 * 10.0mm RF laminated ceramic capacitor and 3.2 * 1.6mm;
(3) the crust piece behind the RF laminated ceramic capacitor printing lamination carries out static pressure such as temperature under 70 ℃, the pressure of 30MPa, carry out the green compact chip cutting then;
(4) RF laminated ceramic capacitor green sintering; Sintering temperature is controlled at 1150～1220 ℃; Temperature rise rate rises to 400 ℃ of temperature rise rates with 1～2 ℃/min from room temperature, 400～1210 ℃ of temperature rise rates with 3～6 ℃/min, soaking time 1.5～4 hours;
(5) RF terminal electrode of multi-layer ceramic capacitor coating sintering adopts 860 ℃ of insulations of resistance furnace 30min.
(6) RF laminated ceramic capacitor product test; Testing tool 4284A, product design size 10.0 * 10.0; Working medium diaphragm thickness 37 * 3,11 layers of the numbers of plies that prints electrode, electrical capacity 3316Pf～3336Pf; Test frequency 1KHZ, DF=0.0001,0.00001,0.000002 are equivalent to Q value>=10000, Q value>=100000, Q value>=500000 and demonstrate ultralow loss. temperature factor (belong to TCC:0 ± 30PPM/ ℃, actual TCC:0+12PPM/ ℃) proof voltage 2000VDC, insulation resistance>=5 * 10
6M; Product design size 2.8 * 2.8; Use identical production batch medium diaphragm thickness 37 * 2,6 layers of the numbers of plies that prints electrode, electrical capacity 149Pf～163Pf; Test frequency 1MHZ, 0.00001,0.000002; Be equivalent to, Q value>=100000, Q value>=500000, proof voltage 1500VDC, insulation resistance>=5 * 10
6M product design size 1.4 * 1.4; Use identical production batch medium diaphragm thickness 37 * 2,5 layers of the numbers of plies that prints electrode, electrical capacity 25Pf～30Pf; Test frequency 1MHZ, DF=0.00001,0.000002; Be equivalent to Q value>=100000, Q value>=500000, proof voltage 500VDC, insulation resistance>=5 * 10
6M;
Measuring result according to embodiment 4 and embodiment 3 shows; The RF laminated ceramic capacitor uses ultra-low loss microwave dielectric ceramic materials and preparation method thereof to make with the RF laminated ceramic capacitor; Reach design objective value in advance, and check and service check through batch curtain coating, the RF laminated ceramic capacitor manufacturing process of a 5KG of medium diaphragm.The ultra-low loss microwave-medium ceramics of obtaining reaches the double goal in the production application of RF electrical condenser.May be used on radio frequency power laminated ceramic capacitor production field; It is domestic scientific and technological autonomous innovation achievement in research in ultra-low loss microwave dielectric ceramic materials preparation field; At zero-temperature coefficient, performance index surmount the successes achieved in research of external ATC company, DIL company in the RF laminated ceramic capacitor products production.Established solid basis to promoting the high-end electronic devices and components development of China, wide market sale and application prospect are arranged, next target gets into industrial large-scale production, and for promoting domestic military, consumer electronic device, the instrument equipment is made contributions.
Claims (4)
1. ultra-low loss microwave-medium ceramics preparation method and the application in the RF electrical condenser; It is characterized in that; The described synthetic in advance piece that burns; The preparation method, form by the Nd of the oxide components of following weight percentage ratio: 50～62wt%, the Ba of 7.1～15wt%, the Ti of 35～45wt%.
2. ultra-low loss microwave-medium ceramics preparation method according to claim 1 and the application in the RF electrical condenser; It is characterized in that; It presses synthetic burning piece in advance, and weight is 1, adds the oxide components of following weight percentage ratio: the Dy of 0.1～5wt%
2O
3, the Nb of 0.1～3.0wt%
2O
5, the Ta of 0.02～1.5wt%
2O
5, the ZrO of 0.05～2.5wt%
2, the Sm of 0.02～1.5wt%
2O
3, the wilkinite of 0.1～5wt%, the MnCO of 0.1～5wt%
3, the above-mentioned at least two or more additives of interpolation etc. are formulated.
3. ultra-low loss microwave-medium ceramics preparation method according to claim 2 and the application in the RF electrical condenser; It is characterized in that; Said ceramics as low-loss microwave medium preparation is adopted and is stirred mill; The ultra-low loss RF condenser dielectric pottery for preparing under production technique and the technology controlling and process key element, wherein the main technique control elements comprises following content:
(1) said microwave dielectric ceramic materials preparation method is characterised in that, by the above-mentioned synthetic in advance piece that burns, is 1 by burning piece weight, adds the following weight percentage composite: the Dy of rare-earth oxidation raw material 0.1～5wt%
2O
3, the Nb of 0.1～3.0wt%
2O
5, the Ta of 0.02～1.5wt%
2O
5, the ZrO of 0.05～2.5wt%
2, the Sm of 0.02～1.5wt%
2O
3, the wilkinite of 0.1～5wt%, the MnCO of 0.1～5wt%
3, add two or more rare earth oxide at least and constitute media ceramic and form, particularly, carry out the weighing preparation according to the weight percentage of the oxide compound of table 1 prescription;
Each oxide raw material weight unit of table 1 is gram
(2) preparation of said microwave-medium ceramics test disk is adopted and is stirred the mill production technique; Be characterised in that; Stipulated that the grinding media material is a zirconia ball; Diameter is that (1～5mm), in ball-milling medium material 4, powder 1, deionized water 0.8～1.5 ratio, stirring consumes time is: stirring in 1～4 hour grinds process program fully;
(3) said trial circle chip capacitor device sintering: being characterised in that, is that the temperature rise rate with 3～6 ℃/min rose to 1130～1200 ℃ again, is incubated 1.5～4 hours, naturally cools to room temperature then after temperature rise rate with 1～2 ℃/min rose to 400 ℃.
4. ultra-low loss microwave-medium ceramics preparation method according to claim 3 and the application in the RF electrical condenser; It is characterized in that; This ultra-low loss microwave dielectric ceramic materials relates to increasing substantially of RF capacitor electrode performance index and comprises following content in the application of RF laminated ceramic capacitor:
>=10000～500000) or higher (1) quality factor: (Q value:; Or loss tangent: tg :≤0.0001～0.000002;
(2) temperature factor: (TCC:0+12PPM/ ℃) or littler;
(3) voltage rating: (UR:500～15000VDC) or higher;
(4) working temperature: (55～125 ℃) expand to 175 ℃ or higher;
(5) K value: 45～55 or higher.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435349A (en) * | 2013-08-09 | 2013-12-11 | 天津大学 | Method for preparing high-quality-factor neodymium niobate dielectric ceramic by means of manganese ion substitution |
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| CN1136026A (en) * | 1996-05-07 | 1996-11-20 | 浙江大学 | HF dielectric ceramics and its manufacture |
| CN1632884A (en) * | 2001-01-10 | 2005-06-29 | 株式会社村田制作所 | Non-reduced dielectric ceramics and ceramic electronic element using the same |
| CN1772698A (en) * | 2005-09-30 | 2006-05-17 | 福州大学 | High-dielectric constant environment friendly microwave dielectric ceramic |
| CN101314545A (en) * | 2008-07-02 | 2008-12-03 | 广东风华高新科技股份有限公司 | Spray coating method for producing dielectric ceramic powder body and obtained products thereof |
-
2010
- 2010-07-28 CN CN2010102389001A patent/CN102336569A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1136026A (en) * | 1996-05-07 | 1996-11-20 | 浙江大学 | HF dielectric ceramics and its manufacture |
| CN1632884A (en) * | 2001-01-10 | 2005-06-29 | 株式会社村田制作所 | Non-reduced dielectric ceramics and ceramic electronic element using the same |
| CN1772698A (en) * | 2005-09-30 | 2006-05-17 | 福州大学 | High-dielectric constant environment friendly microwave dielectric ceramic |
| CN101314545A (en) * | 2008-07-02 | 2008-12-03 | 广东风华高新科技股份有限公司 | Spray coating method for producing dielectric ceramic powder body and obtained products thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103435349A (en) * | 2013-08-09 | 2013-12-11 | 天津大学 | Method for preparing high-quality-factor neodymium niobate dielectric ceramic by means of manganese ion substitution |
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Application publication date: 20120201 |