CN1690014A - Ceramic materials for microwave ceramic capacitor and making method therefor - Google Patents
Ceramic materials for microwave ceramic capacitor and making method therefor Download PDFInfo
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- CN1690014A CN1690014A CN 200410019105 CN200410019105A CN1690014A CN 1690014 A CN1690014 A CN 1690014A CN 200410019105 CN200410019105 CN 200410019105 CN 200410019105 A CN200410019105 A CN 200410019105A CN 1690014 A CN1690014 A CN 1690014A
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- microwave
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- stupalith
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Abstract
The ceramic material for microwave ceramic capacitor has the composition of MgTiO3-CaTiO3, and may be expressed in xMgTiO3-(1-x)CaTiO3, with x being 0.9-1.0. The preparation process includes: mixing basic magnesium carbonate, calcium carbonate and diboron pentoxide in certain proportion, ball milling, stoving, sieving and pre-sintering to obtain fused block; secondary ball milling, stoving, pelletizing, pressing to form and sintering to obtain the ceramic material. The ceramic material for microwave ceramic capacitor has excellent microwave dielectric performance and low cost.
Description
Technical field
The present invention relates to a kind of stupalith and manufacture method thereof that is applied to electronic devices and components, more particularly, is a kind of microwave dielectric ceramic materials and manufacture method thereof.
Background technology
Make rapid progress today of develop rapidly in electronic industry, the integrated and microminiaturized development trend of electronic information technology is just promoting electronics and IT products day by day to slimming, miniaturization, digitizing, multifunction, and highly reliable and cheaply direction develop.Microwave-medium ceramics (MWDC) is the class new function electronic ceramics that year just develops rapidly surplus in the of nearly ten, is bringing into play media isolated in the microwave circuit system, a series of circuit functions such as Medium Wave Guide and dielectric resonance with its excellent micro-wave dielectric character.Microwave-medium ceramics has characteristics such as low-loss, high-k, low frequency temperature coefficient, low thermal coefficient of expansion.The volume problems of too that adopts this material can dwindle wave filter, coupling mechanism, copper rhumbatron in components and parts such as resonator, wave filter, oscillator can solve the integrated problem of microwave device.This material produce maturation can satisfy technology such as contemporary micro-wave communication, mobile communication, satellite communications, broadcast television, radar, electronic countermeasure, guidance to integrated, microminiaturized, highly reliable stabilization of microwave circuit and requirement cheaply.In addition, this class material is dividing quite aspects such as device, shield retaining, signal delay to use in a large number; For example be used for aspects such as millimeter wave communication, radar, surveying instrument.
In China, among microwave-medium ceramics is constantly developing.In low dielectric microwave media ceramic field, for guaranteeing excellent microwave dielectric property, the material cost of employing is higher, makes its widespread use be subjected to certain restriction.
Summary of the invention
The objective of the invention is to overcome the deficiency that prior art exists, the stupalith and the manufacture method of a kind of dielectric properties excellence, microwave ceramic capacitance device cheap for manufacturing cost is provided.
The present invention is realized by following technical proposals, the stupalith of microwave ceramic capacitance device, and its main component is MgTiO
3-CaTiO
3MgTiO wherein
3-CaTiO
3Can use xMgTiO
3-(1-x) CaTiO
3Represent its composition, the x value is 0.9～1.0.This material also contains and accounts for MgTiO
3-CaTiO
3Weight ratio is 0～10% five oxidations, two boron (B
2O
5).
The manufacture method of the stupalith of above-mentioned microwave ceramic capacitance device, its process comprises: to be raw material account for raw material overall weight 45～60%, titanium dioxide according to magnesium basic carbonate accounts for raw material overall weight 35～52%, lime carbonate and account for the mixed that raw material overall weight 0～8%, five oxidations, two boron account for raw material overall weight 0～10% with magnesium basic carbonate, titanium dioxide, lime carbonate, five oxidations, two boron, carry out ball milling, dry, sieve, pre-burning, obtain frit; The frit that obtains is carried out secondary ball milling, oven dry, granulation, compression moulding, carries out sintering and obtain stupalith.The pre-burning of frit is to rise to 1000～1200 ℃ with 5～6 ℃/minute temperature rise rate; Sintering is after rising to 500～550 ℃ with 3 ℃/minute temperature rise rate, rises to 1150～1350 ℃ with 5～6 ℃/minute temperature rise rate again.
The invention has the advantages that prepared stupalith has excellent microwave dielectric property, cost of material is cheap, and sintering can carry out in middle temperature, thereby preparation cost is lower.Stupalith provided by the present invention and manufacture method are a kind of novel stupalith systems, when further reducing dielectric loss, has good thermal stability, cost of material is cheap simultaneously, and sintering can carry out in middle temperature, good market outlook are arranged, can be used as the regeneration product of same type of material.
Embodiment
Embodiment 1:
With analytical pure magnesium basic carbonate, titanium dioxide, lime carbonate, five oxidations, two boron is raw material, according to prescription soda ash formula magnesiumcarbonate 57g, titanium dioxide 41g, lime carbonate 2g, five oxidations, two boron 2g, after these materials mixing, uses ZrO
2Ball added the deionized water ball milling 5 hours, crossed 40 mesh sieves with electrically heated drying cabinet after 120 ℃ of oven dry, carried out pre-burning at 1000～1200 ℃ then, and the pre-burning temperature rise rate is 6 ℃/minute, is incubated 2 hours, obtains frit.Use ZrO again
2Ball and deionized water carry out secondary ball milling (4.5 hours).Mixture behind the ball milling through 120 ℃ of oven dry, add the paraffin granulation, under 80MPa pressure, be pressed into the about 20mm of diameter, the disk shape green compact of the about 1mm of thickness.Green compact carry out sintering at 1150～1350 ℃, and the initial temperature rise rate of sintering process is 3 ℃/minute, rise to 500 ℃ after temperature rise rate become 5.5 ℃/minute, reach sintering temperature after, be incubated 6 hours, furnace cooling 10 hours.Sample burning infiltration silver electrode behind the sintering, welding lead is made the wafer capacitance device.
Utilize Hewlett Packard 4278A Capacitance Meter under 1MHz, to test the electrical capacity C (pF) and the losstangenttan of wafer capacitance device and the relative permittivity ε of calculation medium.Utilize the insulation resistance R (Ω) of Agilent 4339B HighResistance Meter specimen, and the body resistivity ρ of calculation medium
νUtilize GZ-ESPEC thermostat container and HM27002 type electrical condenser C-T characteristic tester Measuring Dielectric Constant temperature factor α
ε
Table 1～table 4 has provided dielectric properties (ε, tan δ, the ρ of preparation sample under different calcined temperatures and sintering temperature respectively
ν, α
ε) measuring result.
Table 1 ε and 0.95MgTiO
3-0.05CaTiO
3The relation of calcined temperature and sintering temperature
Table 2 tan δ (* 10
-4) and 0.95MgTiO
3-0.05CaTiO
3The relation of calcined temperature and sintering temperature
Table 3 α
ε(ppm/ ℃) and 0.95MgTiO
3-0.05CaTiO
3The relation of calcined temperature and sintering temperature
| ??1100℃ ????1150℃ ????1200℃ | ?????-15 ?????-15 ?????-17 | ?????-8 ?????-9 ?????-9 | ????+0 ????+4 ????+5 | ??+1 ??+2 ??+2 | ????+6 ????+7 ????+9 | ????+14 ????+13 ????+16 | ????+22 ????+25 ????+29 |
Table 4 ρ
ν(Ω cm) and 0.95MgTiO
3-0.05CaTiO
3The relation of calcined temperature and sintering temperature
By table 1～table 4 as can be seen, 0.95MgTiO involved in the present invention
3-0.05CaTiO
3Media ceramic, DIELECTRIC CONSTANT and can be regulated ε by changing sintering temperature between 21～25, and general sintering temperature is high more, and ε is big more.Tan δ is generally 1 * 10
-4Below, maximum is no more than 1.4 * 10
-4Tan δ is relevant with calcined temperature and sintering temperature, and in above-mentioned calcined temperature and sintering temperature variation range, the minimum value of tan δ is 0.35 * 10
-4, maximum value is 1.4 * 10
-4, when sintering temperature is low to moderate 1200 ℃, still can obtain very little tan δ value.The temperature coefficient of permittivity α that this is ceramic
εGenerally-15～+ 25ppm/ ℃ between, and have null value, body resistivity ρ
νGreater than 10
13Ω cm.This shows that material of the present invention has two advantages: the one, dielectric properties are good; The 2nd, technology stability is good.
Embodiment 2:
The prescription of sample is all identical with embodiment 1 condition with preparation technology, just changes xMgTiO between 0.9～1.0
3-(1-x) CaTiO
3The x value.Also promptly change the ratio of magnesium basic carbonate in the raw material, titanium dioxide, lime carbonate, five oxidations, two boron.X=0.90, promptly the part by weight of magnesium basic carbonate, titanium dioxide, lime carbonate, five oxidations, two boron is 55: 41: 4: 2; X=0.93, promptly the part by weight of magnesium basic carbonate, titanium dioxide, lime carbonate, five oxidations, two boron is 56: 41: 2.8: 2; X=0.95, promptly the part by weight of magnesium basic carbonate, titanium dioxide, lime carbonate, five oxidations, two boron is 57: 41: 2: 2; X=0.98, promptly the part by weight of magnesium basic carbonate, titanium dioxide, lime carbonate, five oxidations, two boron is 58: 41: 0.8: 2; X=1.0, promptly the part by weight of magnesium basic carbonate, titanium dioxide, lime carbonate, five oxidations, two boron is 59: 41: 0: 2.XMgTiO
3-(1-x) CaTiO
3Calcined temperature is 1100 ℃, and sintering temperature is 1200 ℃.The measuring method of the stupalith parameter that obtains is identical with embodiment 1.Table 5 has provided the rule of the dielectric properties of sample with the variation of x value.
The relation of table 5 sample dielectric properties and x value
| The x value | ????ε | tanδ(×10 -4) | α ε(ppm/℃) | ???ρ ν(Ω·cm) |
| ????0.90 ????0.93 ????0.95 ????0.98 ????1.00 | ????23.7 ????23.7 ????22.2 ????22.5 ????22.4 | ????1.40 ????0.91 ????0.45 ????0.43 ????0.36 | ????+22 ????+13 ????+0 ????-12 ????-35 | ????7.2×10 13????4.1×10 14????5.3×10 14????1.3×10 14????5.4×10 13 |
As can be seen from Table 5, increase the x value, ε is slightly reduced, simultaneously tan δ is reduced.But the x value is 0.95 when following, and tan δ increases to some extent.Change the x value to α
εAlso influential.In the scope that provides in the table, ρ
νAll 10
13More than the Ω cm.
Embodiment 3:
The prescription of sample is all identical with embodiment 1 condition with preparation technology, just changes 0.95MgTiO
3-0.05CaTiO
3The middle B that adds
2O
5Weight ratio, make B
2O
5Weight percent in 0～10% scope, change.Calcined temperature is 1100 ℃, and sintering temperature is 1200 ℃.The measuring method of the stupalith parameter that obtains is identical with embodiment 1.Table 6 has provided the dielectric properties of sample with B
2O
5The rule of content.
Table 6 sample dielectric properties and B
2O
5The relation of content
| Sample number into spectrum | Optimal sintering temperature | Every 100g 0.95MgTiO 3- ?0.05CaTiO 3Add B 2O 5(g) | ????ε | ????tanδ ????(×10 -4) | ????α ε(ppm/℃) | ????ρ ν(Ω·cm) |
| ????1# ????2# ????3# ????4# ????5# | ?1300℃ ??1260℃ ??1200℃ ??1180℃ ??1150℃ | ????0 ????2 ????5 ????8 ????10 | ???22.1 ???22.0 ???22.2 ???21.2 ???19.8 | ?????0.41 ?????0.40 ?????0.45 ?????0.47 ?????0.56 | ?????+9 ?????+5 ?????+0 ?????-7 ?????-11 | ????4.9×10 13????3.1×10 14????4.7×10 14????4.6×10 14????2.9×10 14 |
As can be seen from Table 6, increase MgTiO
3-CaTiO
3B in the media ceramic
2O
5Content, the optimal sintering temperature of sample is significantly reduced, and simultaneously ε descends slightly, it is less that tan δ keeps, temperature factor is tending towards negative value.In the scope that provides in the table, ρ
νAll 10
13More than the cm.
Claims (3)
1. the stupalith of a microwave ceramic capacitance device is characterized in that, described material comprises MgTiO
3-CaTiO
3Compound, wherein MgTiO
3-CaTiO
3Can use xMgTiO
3-(1-x) CaTiO
3Represent its composition, the x value is 0.9～1.0.
2. the stupalith of microwave ceramic capacitance device according to claim 1 is characterized in that, described material also contains and accounts for MgTiO
3-CaTiO
3Weight ratio is 0～10% five oxidations, two boron.
3. a method of ceramic material for preparing microwave ceramic capacitance device as claimed in claim 1 is characterized in that, comprises the steps:
(1) be raw material with magnesium basic carbonate, titanium dioxide, lime carbonate, five oxidations, two boron, accounting for raw material overall weight 45～60%, titanium dioxide according to magnesium basic carbonate accounts for raw material overall weight 35～52%, lime carbonate and accounts for the mixed that raw material overall weight 0～8%, five oxidations, two boron account for raw material overall weight 0～10%
(2) carry out ball milling, dry, sieve, pre-burning rises to 1000～1200 ℃ with 5～6 ℃/minute temperature rise rate, obtains frit;
(3) frit that obtains is carried out secondary ball milling, oven dry, granulation, compression moulding,
(4) carry out sintering then, rise to 500～550 ℃ with 3 ℃/minute temperature rise rates after, rise to 1150～1350 ℃ with 5～6 ℃/minute temperature rise rate again, obtain stupalith at last.
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|---|---|---|---|
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153343A (en) * | 2011-01-10 | 2011-08-17 | 天津大学 | Method for preparing high Q-value magnesium titanate base microwave medium ceramics by adopting reactive sintering method |
| CN103588477A (en) * | 2013-11-28 | 2014-02-19 | 云南云天化股份有限公司 | Microwave dielectric ceramic powder and preparation method thereof |
| CN109279892A (en) * | 2018-11-21 | 2019-01-29 | 湖北天瓷电子材料有限公司 | A method of microwave ceramics pre-burning powder is prepared using coprecipitation |
| CN110256066A (en) * | 2019-04-30 | 2019-09-20 | 天津大学 | A kind of intermediate sintering temperature microwave dielectric material that frequency-temperature characteristic is excellent |
| CN111004030A (en) * | 2019-12-24 | 2020-04-14 | 苏州同拓光电科技有限公司 | MgTiO (magnesium-titanium-oxide) powder3Microwave-based dielectric ceramic and preparation method thereof |
| CN111704460A (en) * | 2020-05-25 | 2020-09-25 | 广东风华高新科技股份有限公司 | MgTiO for NP0 type MLCC3Base radio frequency ceramic powder and preparation method thereof |
| CN112624755A (en) * | 2020-12-02 | 2021-04-09 | 无锡市高宇晟新材料科技有限公司 | Microwave dielectric ceramic material and preparation method thereof |
| CN113979744A (en) * | 2021-10-26 | 2022-01-28 | 西南科技大学 | Magnesium-calcium-titanium microwave dielectric ceramic powder and preparation method and application thereof |
| CN114988866A (en) * | 2022-04-18 | 2022-09-02 | 浙江钛迩赛新材料有限公司 | 5G ceramic filter material, low-temperature sintering method and application thereof |
-
2004
- 2004-04-30 CN CN 200410019105 patent/CN1690014A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153343A (en) * | 2011-01-10 | 2011-08-17 | 天津大学 | Method for preparing high Q-value magnesium titanate base microwave medium ceramics by adopting reactive sintering method |
| CN103588477A (en) * | 2013-11-28 | 2014-02-19 | 云南云天化股份有限公司 | Microwave dielectric ceramic powder and preparation method thereof |
| CN109279892A (en) * | 2018-11-21 | 2019-01-29 | 湖北天瓷电子材料有限公司 | A method of microwave ceramics pre-burning powder is prepared using coprecipitation |
| CN110256066A (en) * | 2019-04-30 | 2019-09-20 | 天津大学 | A kind of intermediate sintering temperature microwave dielectric material that frequency-temperature characteristic is excellent |
| CN111004030A (en) * | 2019-12-24 | 2020-04-14 | 苏州同拓光电科技有限公司 | MgTiO (magnesium-titanium-oxide) powder3Microwave-based dielectric ceramic and preparation method thereof |
| CN111004030B (en) * | 2019-12-24 | 2021-09-07 | 苏州同拓光电科技有限公司 | MgTiO (magnesium-titanium-oxide) powder3Microwave-based dielectric ceramic and preparation method thereof |
| CN111704460A (en) * | 2020-05-25 | 2020-09-25 | 广东风华高新科技股份有限公司 | MgTiO for NP0 type MLCC3Base radio frequency ceramic powder and preparation method thereof |
| CN112624755A (en) * | 2020-12-02 | 2021-04-09 | 无锡市高宇晟新材料科技有限公司 | Microwave dielectric ceramic material and preparation method thereof |
| CN113979744A (en) * | 2021-10-26 | 2022-01-28 | 西南科技大学 | Magnesium-calcium-titanium microwave dielectric ceramic powder and preparation method and application thereof |
| CN113979744B (en) * | 2021-10-26 | 2022-10-18 | 西南科技大学 | Magnesium-calcium-titanium microwave dielectric ceramic powder and preparation method and application thereof |
| CN114988866A (en) * | 2022-04-18 | 2022-09-02 | 浙江钛迩赛新材料有限公司 | 5G ceramic filter material, low-temperature sintering method and application thereof |
| CN114988866B (en) * | 2022-04-18 | 2023-10-13 | 浙江钛迩赛新材料有限公司 | 5G ceramic filter material, low-temperature sintering method and application thereof |
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