CN100455539C - Microwave dielectric ceramic and its prepn - Google Patents

Microwave dielectric ceramic and its prepn Download PDF

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Publication number
CN100455539C
CN100455539C CNB2006100408919A CN200610040891A CN100455539C CN 100455539 C CN100455539 C CN 100455539C CN B2006100408919 A CNB2006100408919 A CN B2006100408919A CN 200610040891 A CN200610040891 A CN 200610040891A CN 100455539 C CN100455539 C CN 100455539C
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raw material
preparation
temperature
burning
sintering
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CN1887793A (en
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张其土
张校平
李斌
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Nanjing Tech University
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Abstract

The present invention relates to microwave ceramic dielectric material, and is especially one kind of serial BaO-Y2O3-TiO2 microwave ceramic dielectric materials for mobile communication dielectric antenna, filter, module and other RF elements and devices and their preparation process. The serial BaO-Y2O3-TiO2 microwave ceramic dielectric materials are prepared with the raw materials including BaCO3, Y2O3 and TiO2, and through mixing in certain weight proportion, ball milling, stoving, pre-sintering, ball milling for the second time, pelletizing, sieving, pressing to form and sintering. The serial BaO-Y2O3-TiO2 microwave ceramic dielectric materials have excellent dielectric performance, relatively low sintering temperature, no environmental pollution, low cost and other advantages.

Description

A kind of microwave-medium ceramics and preparation method thereof
Technical field
The present invention relates to the microwave-medium ceramics and the preparation method of radio frequency components and parts such as tracking exchage polyrod antenna, wave filter and module; Relate in particular to a kind of serial BaO-Y2O3-TiO2 microwave-medium ceramics and preparation method thereof.
Background technology
Microwave-medium ceramics is widely used in many fields of microwave technology, as mobile telephone, telestar receptor, military radar, wireless remote control etc.Along with mobile communication gets fast development, mobile communication terminal is just towards miniaturization, lightweight, integrated direction development in recent years.The stupalith of low temperature system more and more is subject to people's attention.Study maximum BaO-Sm at present 2O 3-TiO 2System, BaO-Nd 2O 3-TiO 2System waits microwave-medium ceramics ε rBe about 50～80, Qf 〉=4000, but intrinsic sintering temperature is than higher (being about 1340 ℃～1400 ℃), and rare earths materials such as Sm, Nd are relatively more expensive, cause product price higher, are not suitable for popular the popularization.BaO-B 2O 3-SiO 2-TiO 2The system (patent No. CN1559981) though microwave-medium ceramics sintering temperature lower (about 950 ℃), ε rHave only 4～50, be not suitable for the demand for development of microwave technical field.
Summary of the invention
Technical problem to be solved by this invention is in order to overcome the intrinsic sintering temperature of prior art than higher, though or the low ε of sintering temperature rThe shortcoming that value is low and proposed the relatively lower BaO-Y of the relatively good and intrinsic temperature of a kind of dielectric properties 2O 3-TiO 2Series microwave dielectric ceramic; Another object of the present invention has also proposed the preparation method of above-mentioned microwave-medium ceramics.
Technical scheme of the present invention is: it is as follows that a kind of microwave dielectric ceramic materials, its material component and each component account for the molar percentage of raw material total amount:
The material component molar percentage
BaCO 3 10～20％
Y 2O 3 14～33％
TiO 2 57～72％
The present invention also provides the preparation method of above-mentioned microwave dielectric ceramic materials, and its step is as follows:
A, take by weighing raw material in above-mentioned raw materials component ratio; The raw material that weighs up ball milling 16～24 hours on ball mill, oven dry again;
The pre-burning that heats up after B, the raw material stoving is reduced to 18 ℃～25 ℃ with stove then; The pellet of pre-burning was ground 5～8 hours;
C, in the powder that above-mentioned ball milling is crossed, add the PVA binding agent, grind granulation about 1～3 hour then, sieve, and with powder compression moulding;
D, forming composition is heated up, sintering and insulation are reduced to 18 ℃～25 ℃ with stove then.
Wherein ball mill is preferably the roller milling machine in the steps A, adopts wet ball grinding.3～3.5 ℃/min of temperature rise rate among the step B, calcined temperature are 900 ℃～1150 ℃, and the pre-burning time is 2h～8h.
The add-on of PVA binding agent is the 7～10wt% that accounts for raw materials quality among the step C.Sieve among the step C with 80 mesh sieve, the general compression moulding of powder is thin rounded flakes.3～3.5 ℃/min of temperature rise rate among the step D, sintering temperature is 1220～1280 ℃, soaking time 2h～8h.
Beneficial effect:
1. BaO-Y of the present invention 2O 3-TiO 2Series microwave dielectric ceramic dielectric properties (ε rBe about 50～84, Qf 〉=4000) suitable with other prescription series, but intrinsic sintering temperature lower (1220 ℃～1280 ℃) greatly reduces energy consumption, is fit to low sintering research, helps the development and the application of new low temperature system microwave-medium ceramics.
2. compliance with environmental protection requirements of the present invention, nontoxicity, environmentally safe, and Y 2O 3Price is more cheap with respect to the rare earth of other system, and marketable value is arranged.
3. the present invention helps improving the comprehensive utilization ratio of rare earth resources, slows down Y 2O 3The surplus relatively of rare earth oxide.
Embodiment
The invention will be further described below in conjunction with embodiment, but should not limit protection scope of the present invention with this.
The composition of 9 specific embodiments of serial BaO-Y2O3-TiO2 microwave dielectric ceramic materials of the present invention is as shown in table 1:
Table 1
Figure C20061004089100041
Embodiment 1 #:
Form as in the table 11 #Shown in, concrete preparation method comprises the following steps:
1. calculate the weight percent of raw material by the molar percentage (mol%) of the composition of selecting raw material, take by weighing raw material then.
2. the sample that weighs up is placed ball grinder, wet ball grinding 24 hours.
3. after the raw material stoving in 1150 ℃, air atmosphere pre-burning 2h, 3.5 ℃/min of temperature rise rate lowers the temperature with stove then.
4. with the material of pre-burning, wet ball grinding 6 hours (300 rev/mins) on planetary mills.
5. the ratio adding concentration in 7wt% is the PVA binding agent of 7wt%, grinds granulation in about 1 hour in agate mortar, crosses 80 mesh sieves.
6. the powder that will be mixed with 7wt%PVA with powder compressing machine is pressed into thick one by one about 3mm, and the thin discs of diameter 13mm, pressure are about 100MPa.
7. with disk at 1280 ℃, sintering in the air atmosphere, 3 ℃/min of temperature rise rate, soaking time 2h lowers the temperature with stove then.
Test result to this microwave dielectric ceramic materials is as follows:
With the sample surfaces polishing, adopt Agilient 8722ET network analyzer, measure DIELECTRIC CONSTANT according to the Hakki-Coleman method rAnd quality factor q.Temperature coefficient of resonance frequency is according to formula τ f = f 2 - f 1 f 1 ( T 2 - T 1 ) Calculate.Dielectric properties are as follows: ε r=79, Qf=4083, τ f=-28ppm/ ℃
Embodiment 2 #:
Form as in the table 11 #Shown in, concrete preparation method comprises the following steps:
1. calculate the weight percent of raw material by the molar percentage (mol%) of the composition of selecting raw material, take by weighing raw material then.
2. the sample that weighs up is placed ball grinder, wet ball grinding 24 hours.
3. after the raw material stoving in 900 ℃, air atmosphere pre-burning 2h, 3.5 ℃/min of temperature rise rate lowers the temperature with stove then.
4. with the material of pre-burning, wet ball grinding 6 hours (300 rev/mins) on planetary mills.
5. the ratio adding concentration in 7wt% is the PVA binding agent of 7wt%, grinds granulation in about 1 hour in agate mortar, crosses 80 mesh sieves.
6. the powder that will be mixed with 7wt%PVA with powder compressing machine is pressed into thick one by one about 3mm, and the thin discs of diameter 13mm, pressure are about 100MPa.
7. with disk at 1270 ℃, sintering in the air atmosphere, 3 ℃/min of temperature rise rate, soaking time 2h lowers the temperature with stove then.
Test result to this microwave dielectric ceramic materials is as follows:
With the sample surfaces polishing, adopt Agilient 8722ET network analyzer, measure DIELECTRIC CONSTANT according to the Hakki-Coleman method rAnd quality factor q.Temperature coefficient of resonance frequency is according to formula τ f = f 2 - f 1 f 1 ( T 2 - T 1 ) Calculate.Dielectric properties are as follows: ε r=50, Qf=4333, τ f=-15ppm/ ℃
Embodiment 3 #:
Form as in the table 11 #Shown in, concrete preparation method comprises the following steps:
1. calculate the weight percent of raw material by the molar percentage (mol%) of the composition of selecting raw material, take by weighing raw material then.
2. the sample that weighs up is placed ball grinder, wet ball grinding 24 hours.
3. after the raw material stoving in 1000 ℃, air atmosphere pre-burning 2h, 3.5 ℃/min of temperature rise rate lowers the temperature with stove then.
4. with the material of pre-burning, wet ball grinding 6 hours (300 rev/mins) on planetary mills.
5. the ratio adding concentration in 7wt% is the PVA binding agent of 7wt%, grinds granulation in about 1 hour in agate mortar, crosses 80 mesh sieves.
6. the powder that will be mixed with 7wt%PVA with powder compressing machine is pressed into thick one by one about 3mm, and the thin discs of diameter 13mm, pressure are about 100MPa.
7. with disk at 1240 ℃, sintering in the air atmosphere, 3 ℃/min of temperature rise rate, soaking time 2h lowers the temperature with stove then.
Test result to this microwave dielectric ceramic materials is as follows:
With the sample surfaces polishing, adopt Agilient 8722ET network analyzer, measure DIELECTRIC CONSTANT according to the Hakki-Coleman method rAnd quality factor q.Temperature coefficient of resonance frequency is according to formula τ f = f 2 - f 1 f 1 ( T 2 - T 1 ) Calculate.Dielectric properties are as follows: ε r=80, Qf=5500, τ f=11ppm/ ℃
Embodiment 4 #:
Form as in the table 11 #Shown in, concrete preparation method comprises the following steps:
1. calculate the weight percent of raw material by the molar percentage (mol%) of the composition of selecting raw material, take by weighing raw material then.
2. the sample that weighs up is placed ball grinder, wet ball grinding 24 hours.
3. after the raw material stoving in 1050 ℃, air atmosphere pre-burning 2h, 3.5 ℃/min of temperature rise rate lowers the temperature with stove then.
4. with the material of pre-burning, wet ball grinding 6 hours (300 rev/mins) on planetary mills.
5. the ratio adding concentration in 7wt% is the PVA binding agent of 7wt%, grinds granulation in about 1 hour in agate mortar, crosses 80 mesh sieves.
6. the powder that will be mixed with 7wt%PVA with powder compressing machine is pressed into thick one by one about 3mm, and the thin discs of diameter 13mm, pressure are about 100MPa.
7. with disk at 1240 ℃, sintering in the air atmosphere, 3 ℃/min of temperature rise rate, soaking time 2h lowers the temperature with stove then.
Test result to this microwave dielectric ceramic materials is as follows:
With the sample surfaces polishing, adopt Agilient 8722ET network analyzer, measure DIELECTRIC CONSTANT according to the Hakki-Coleman method rAnd quality factor q.Temperature coefficient of resonance frequency is according to formula τ f = f 2 - f 1 f 1 ( T 2 - T 1 ) Calculate.Dielectric properties are as follows: ε r=58, Qf=8300, τ f=9ppm/ ℃
Embodiment 5 #:
Form as in the table 11 #Shown in, concrete preparation method comprises the following steps:
1. calculate the weight percent of raw material by the molar percentage (mol%) of the composition of selecting raw material, take by weighing raw material then.
2. the sample that weighs up is placed ball grinder, wet ball grinding 24 hours.
3. after the raw material stoving in 1100 ℃, air atmosphere pre-burning 2h, 3.5 ℃/min of temperature rise rate lowers the temperature with stove then.
4. with the material of pre-burning, wet ball grinding 6 hours (300 rev/mins) on planetary mills.
5. the ratio adding concentration in 7wt% is the PVA binding agent of 7wt%, grinds granulation in about 1 hour in agate mortar, crosses 80 mesh sieves.
6. the powder that will be mixed with 7wt%PVA with powder compressing machine is pressed into thick one by one about 3mm, and the thin discs of diameter 13mm, pressure are about 100MPa.
7. with disk at 1250 ℃, sintering in the air atmosphere, 3 ℃/min of temperature rise rate, soaking time 2h lowers the temperature with stove then.
Test result to this microwave dielectric ceramic materials is as follows:
With the sample surfaces polishing, adopt Agilient 8722ET network analyzer, measure DIELECTRIC CONSTANT according to the Hakki-Coleman method rAnd quality factor q.Temperature coefficient of resonance frequency is according to formula τ f = f 2 - f 1 f 1 ( T 2 - T 1 ) Calculate.Dielectric properties are as follows: ε r=65, Qf=8520, τ f=10ppm/ ℃
Embodiment 6 #:
Form as in the table 11 #Shown in, concrete preparation method comprises the following steps:
1. calculate the weight percent of raw material by the molar percentage (mol%) of the composition of selecting raw material, take by weighing raw material then.
2. the sample that weighs up is placed ball grinder, wet ball grinding 24 hours.
3. after the raw material stoving in 1100 ℃, air atmosphere pre-burning 2h, 3.5 ℃/min of temperature rise rate lowers the temperature with stove then.
4. with the material of pre-burning, wet ball grinding 6 hours (300 rev/mins) on planetary mills.
5. the ratio adding concentration in 7wt% is the PVA binding agent of 7wt%, grinds granulation in about 1 hour in agate mortar, crosses 80 mesh sieves.
6. the powder that will be mixed with 7wt%PVA with powder compressing machine is pressed into thick one by one about 3mm, and the thin discs of diameter 13mm, pressure are about 100MPa.
7. with disk at 1240 ℃, sintering in the air atmosphere, 3 ℃/min of temperature rise rate, soaking time 2h lowers the temperature with stove then.
Test result to this microwave dielectric ceramic materials is as follows:
With the sample surfaces polishing, adopt Agilient 8722ET network analyzer, measure DIELECTRIC CONSTANT according to the Hakki-Coleman method rAnd quality factor q.Temperature coefficient of resonance frequency is according to formula τ f = f 2 - f 1 f 1 ( T 2 - T 1 ) Calculate.Dielectric properties are as follows: ε r=57, Qf=7200, τ f=9ppm/ ℃
Embodiment 7 #:
Form as in the table 11 #Shown in, concrete preparation method comprises the following steps:
1. calculate the weight percent of raw material by the molar percentage (mol%) of the composition of selecting raw material, take by weighing raw material then.
2. the sample that weighs up is placed ball grinder, wet ball grinding 24 hours.
3. after the raw material stoving in 1050 ℃, air atmosphere pre-burning 2h, 3.5 ℃/min of temperature rise rate lowers the temperature with stove then.
4. with the material of pre-burning, wet ball grinding 6 hours (300 rev/mins) on planetary mills.
5. the ratio adding concentration in 7wt% is the PVA binding agent of 7wt%, grinds granulation in about 2 hours in agate mortar, crosses 80 mesh sieves.
6. the powder that will be mixed with 7wt%PVA with powder compressing machine is pressed into thick one by one about 3mm, and the thin discs of diameter 13mm, pressure are about 100MPa.
7. with disk at 1280 ℃, sintering in the air atmosphere, 3 ℃/min of temperature rise rate, soaking time 2h lowers the temperature with stove then.
Test result to this microwave dielectric ceramic materials is as follows:
With the sample surfaces polishing, adopt Agilient 8722ET network analyzer, measure DIELECTRIC CONSTANT according to the Hakki-Coleman method rAnd quality factor q.Temperature coefficient of resonance frequency is according to formula τ f = f 2 - f 1 f 1 ( T 2 - T 1 ) Calculate.Dielectric properties are as follows: ε r=60, Qf=5000, τ f=50ppm/ ℃
Embodiment 8 #:
Composition is shown in 1# in the table 1, and concrete preparation method comprises the following steps:
1. calculate the weight percent of raw material by the molar percentage (mol%) of the composition of selecting raw material, take by weighing raw material then.
2. the sample that weighs up is placed ball grinder, wet ball grinding 24 hours.
3. after the raw material stoving in 1150 ℃, air atmosphere pre-burning 2h, 3.5 ℃/min of temperature rise rate lowers the temperature with stove then.
4. with the material of pre-burning, wet ball grinding 6 hours (300 rev/mins) on planetary mills.
5. the ratio adding concentration in 7wt% is the PVA binding agent of 7wt%, grinds granulation in about 3 hours in agate mortar, crosses 80 mesh sieves.
6. the powder that will be mixed with 7wt%PVA with powder compressing machine is pressed into thick one by one about 3mm, and the thin discs of diameter 13mm, pressure are about 100MPa.
7. with disk at 1220 ℃, sintering in the air atmosphere, 3 ℃/min of temperature rise rate, soaking time 2h lowers the temperature with stove then.
Test result to this microwave dielectric ceramic materials is as follows:
With the sample surfaces polishing, adopt Agilient 8722ET network analyzer, measure DIELECTRIC CONSTANT according to the Hakki-Coleman method rAnd quality factor q.Temperature coefficient of resonance frequency is according to formula τ f = f 2 - f 1 f 1 ( T 2 - T 1 ) Calculate.Dielectric properties are as follows: ε r=78, Qf=5250, τ f=22ppm/ ℃
Embodiment 9 #:
Form as in the table 11 #Shown in, concrete preparation method comprises the following steps:
1. calculate the weight percent of raw material by the molar percentage (mol%) of the composition of selecting raw material, take by weighing raw material then.
2. the sample that weighs up is placed ball grinder, wet ball grinding 24 hours.
3. after the raw material stoving in 1150 ℃, air atmosphere pre-burning 2h, 3.5 ℃/min of temperature rise rate lowers the temperature with stove then.
4. with the material of pre-burning, wet ball grinding 6 hours (300 rev/mins) on planetary mills.
5. the ratio adding concentration in 7wt% is the PVA binding agent of 7wt%, grinds granulation in about 3 hours in agate mortar, crosses 80 mesh sieves.
6. the powder that will be mixed with 7wt%PVA with powder compressing machine is pressed into thick one by one about 3mm, and the thin discs of diameter 13mm, pressure are about 100MPa.
7. with disk at 1260 ℃, sintering in the air atmosphere, 3 ℃/min of temperature rise rate, soaking time 2h lowers the temperature with stove then.
Test result to this microwave dielectric ceramic materials is as follows:
With the sample surfaces polishing, adopt Agilient 8722ET network analyzer, measure DIELECTRIC CONSTANT according to the Hakki-Coleman method rAnd quality factor q.Temperature coefficient of resonance frequency is according to formula τ f = f 2 - f 1 f 1 ( T 2 - T 1 ) Calculate.Dielectric properties are as follows: ε r=62, Qf=7142, τ f=16ppm/ ℃

Claims (7)

1, a kind of microwave dielectric ceramic materials, its raw material is formed and each component to account for the molar percentage of raw material total amount as follows:
The material component molar percentage
BaCO 3 10～20％
Y 2O 3 14～33％
TiO 2 57～72％。
2, a kind of preparation method of microwave dielectric ceramic materials as claimed in claim 1, its step is as follows:
A, take by weighing raw material in the ratio of claim 1; The raw material that weighs up ball milling 16～24 hours on ball mill, oven dry again;
The pre-burning that heats up after B, the raw material stoving is reduced to 18 ℃～25 ℃ with stove then; The pellet of pre-burning was ground 5～8 hours;
C, in the powder that above-mentioned ball milling is crossed, add the PVA binding agent, grind granulation in 1～3 hour then, sieve, and with powder compression moulding;
D, forming composition is heated up, sintering and insulation are reduced to 18 ℃～25 ℃ with stove then.
3, preparation method according to claim 2 is characterized in that ball mill is the roller milling machine in the steps A, adopts wet ball grinding.
4, preparation method according to claim 2 is characterized in that 3～3.5 ℃/min of temperature rise rate among the step B, and calcined temperature is 900 ℃～1150 ℃, and the pre-burning time is 2h～8h.
5, preparation method according to claim 2, the add-on that it is characterized in that PVA binding agent among the step C is the 7～10wt% that accounts for raw materials quality.
6, preparation method according to claim 2 is characterized in that sieving among the step C with 80 mesh sieve, and powder compression moulding is thin rounded flakes.
7, preparation method according to claim 2 is characterized in that 3～3.5 ℃/min of temperature rise rate among the step D, and sintering temperature is 1220～1280 ℃, soaking time 2h～8h.
CNB2006100408919A 2006-08-02 2006-08-02 Microwave dielectric ceramic and its prepn Expired - Fee Related CN100455539C (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102659408A (en) * 2012-05-23 2012-09-12 南京工业大学 La2O3-TiO2 system microwave medium ceramic and preparation method thereof

Citations (7)

* Cited by examiner, † Cited by third party
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
CN1212439A (en) * 1997-09-25 1999-03-31 株式会社村田制作所 Dielectric ceramic composition and monolithic ceramic capacitor using composition
CN1244514A (en) * 1998-08-11 2000-02-16 株式会社村田制作所 Dielectric ceramic composition and laminated ceramic capacitor with said composition
CN1247843A (en) * 1998-09-11 2000-03-22 株式会社村田制作所 Dielectric ceramic composition and laminated ceramic element
CN1360320A (en) * 2000-12-19 2002-07-24 株式会社村田制作所 Synthetic multi-layer ceramic electronic component and mfg. method thereof
CN1445792A (en) * 2002-03-15 2003-10-01 株式会社村田制作所 Dielectric ceramic composite and its making method, and laminated capacitor
CN1208783C (en) * 2000-07-21 2005-06-29 株式会社村田制作所 Dielectric ceramic composition

Patent Citations (7)

* Cited by examiner, † Cited by third party
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
CN1212439A (en) * 1997-09-25 1999-03-31 株式会社村田制作所 Dielectric ceramic composition and monolithic ceramic capacitor using composition
CN1244514A (en) * 1998-08-11 2000-02-16 株式会社村田制作所 Dielectric ceramic composition and laminated ceramic capacitor with said composition
CN1247843A (en) * 1998-09-11 2000-03-22 株式会社村田制作所 Dielectric ceramic composition and laminated ceramic element
CN1208783C (en) * 2000-07-21 2005-06-29 株式会社村田制作所 Dielectric ceramic composition
CN1360320A (en) * 2000-12-19 2002-07-24 株式会社村田制作所 Synthetic multi-layer ceramic electronic component and mfg. method thereof
CN1445792A (en) * 2002-03-15 2003-10-01 株式会社村田制作所 Dielectric ceramic composite and its making method, and laminated capacitor

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