WO2006137153A1 - 電子デバイス用誘電体磁器組成物 - Google Patents
電子デバイス用誘電体磁器組成物 Download PDFInfo
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- WO2006137153A1 WO2006137153A1 PCT/JP2005/011651 JP2005011651W WO2006137153A1 WO 2006137153 A1 WO2006137153 A1 WO 2006137153A1 JP 2005011651 W JP2005011651 W JP 2005011651W WO 2006137153 A1 WO2006137153 A1 WO 2006137153A1
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Definitions
- the present invention relates to a dielectric ceramic composition having optimal characteristics for microwave electronic devices used for dielectric resonators, dielectric filters, phase shifters, etc.
- the present invention relates to a novel dielectric ceramic composition for electronic devices in which a solid solution of Ga 2 -Sr oxide and / or a solid solution of A ⁇ Ga oxide and Sr oxide exist.
- Dielectric porcelain compositions are widely used in electronic devices intended for high frequency regions such as microwaves and millimeter waves.
- the characteristics required for these applications include:
- Non-patent Document 1 La-Ti-ATi 0 system
- ⁇ r 36
- Qf Value 45,000GHz
- Patent Document 3 It has been proposed to improve the Qf value by including 2 3 (Patent Document 3). Although this material has excellent properties with Qf value of 30,000 or more, ⁇ 1 ⁇ positive or negative is relatively large It has become a value.
- Patent Document 4 We have proposed a dielectric ceramic composition for microwaves (Patent Document 4). This composition improves the Qf value of a La-A ⁇ Sr-Ti oxide by adding a specific amount of Ga.
- Non-Patent Document l Japan, J. appl, phys, Vol. 36 (1997) 6814
- Non-Patent Document 2 Electronic Ceramics September 1993, page 3
- Patent Document 1 Japanese Patent No. 2625074
- Patent Document 2 Japanese Patent Laid-Open No. 11-130528
- Patent Document 3 Japanese Patent Laid-Open No. 11-106255
- Patent Document 4 WO 02/36519 A1 Publication
- This invention has a high Qf value in the vicinity of a relative dielectric constant ⁇ r of 39, and the temperature of the resonance frequency.
- An object of the present invention is to provide a dielectric ceramic composition for electronic devices having a dielectric property that is small in coefficient ⁇ i3 ⁇ 4 and whose value can be controlled in a wide range in the positive and negative directions.
- the inventors of the present invention have found that in a La-A-to-Sr-Ti-based oxide, the temperature coefficient of the resonance frequency is reduced by 1 ⁇ and the value can be controlled over a wide range in the positive and negative directions.
- the composition was intensively studied.
- the inventors reduced the content of each element to a specific range and replaced a part of Sr with Ca.
- a solid solution of a-based oxide and a structure with precipitated Sr oxide were obtained, and in particular, when the relative dielectric constant ⁇ r is around 39, it has a high Qf value of 57,000 or more, and the resonance frequency Temperature coefficient of ⁇ ⁇
- the present invention was completed by discovering that it can be controlled in the range of -8 ppm / ° C to 6 ppm / ° C.
- the present invention relates to (l-x) (La Ln) (A1 Ga) 0 -x (Sr Ca) TiO solid solution (however, L
- n is at least one of Pr and Nd, and x, y, z, and m satisfy the following values) as a main phase, and a solid solution of AH3 a-Sr oxide or A ⁇ Ga oxide at the grain boundary And a Sr oxide, or a solid solution of A ⁇ Ga-Sr oxide and a solid solution of A ⁇ Ga oxide and a Sr oxide.
- ⁇ - ⁇ 0 is substantially absent at the grain boundary.
- a dielectric ceramic composition for electronic devices is provided.
- the relative dielectric constant ⁇ r is around 39
- Qf value is 57,000 or more and temperature coefficient of resonance frequency ⁇ -8ppm / ° C to 6ppm / ° C o
- a part of Sr is replaced with Ca, whereby the temperature coefficient is controlled.
- the reactivity at the time of calcination is improved, and calcination is performed at a temperature of 1200 ° C to 1300 ° C, which was difficult with conventional La-A ⁇ Sr-Ti-based oxide dielectric ceramics. It becomes possible to do.
- the dielectric ceramic composition according to the present invention comprises (1-x) (La Ln) (A1 Ga) 0-x (SrCa) TiO.
- Ln is at least one of Pr and Nd, or There are two types. Ln can be moved ⁇ 13 ⁇ 4 in the positive direction by using Pr, and ⁇ can be moved in the negative direction by using Nd.
- X indicates the component range of (La Ln) (Al Ga) 0 as (l-x), and the component range of (Sr Ca) TiO as (x).
- 0.5 ⁇ x ⁇ 0.6 is a preferable range. If X is less than 0.5, the relative permittivity ⁇ r decreases, and if it exceeds 0.6, the relative permittivity ⁇ r increases, and the Qf value decreases to less than 57,000.
- y represents a component range of La and Ln, and 0 ⁇ y ⁇ 0.2 is a preferable range. If y exceeds 0.2, the Qf value decreases and increases by 1 ⁇ , which is not preferable.
- z represents a component range of A1 and Ga, and 0 ⁇ z ⁇ 0.05 is a preferable range. If z exceeds 0.05, the Qf value decreases, which is not preferable. In particular, Ga in this invention is very important.
- the zero value is low and ⁇ f cannot be controlled.
- m represents a component range of Sr and Ca, and 0 ⁇ m ⁇ 0.3 is a preferable range. If m exceeds 0.3, ⁇ ⁇ ⁇ becomes too large, which is not preferable.
- the temperature coefficient can be controlled and the reactivity during calcination can be improved.
- the presence of the grain boundary can be confirmed by EPMA analysis of the sintered body of the dielectric ceramic composition.
- all of the Sr oxides are not contained in the main phase, the force that exists as a solid solution of A ⁇ Ga-Sr oxides at the grain boundaries, the A ⁇ Ga oxides
- the above (1) to (3) are limited because it is difficult to distinguish between the solid solution and the Sr oxide.
- the dielectric ceramic composition of the present invention it is clear that at least A1 forms a solid solution of Ga and oxide and exists at the grain boundaries as demonstrated by the examples described later. Therefore, in this porcelain composition, A1 does not exist as ⁇ - ⁇ 0, so ⁇ - ⁇ 10 is substantially
- the method for producing a dielectric ceramic composition of the present invention includes raw material powder blending, wet or dry mixing, drying, calcining, wet or dry grinding, drying, granulation, molding, sintering, and each step. It can be easily manufactured by obtaining a sintered body by a known method of appropriately selecting an apparatus.
- Purity powder was prepared. Each powder was blended as shown in Table 1, mixed in pure water and dried to obtain a mixed powder having an average particle size of 0.7 to 1.4 ⁇ m.
- the mixed powder was calcined at 1100 ° C. to 1300 ° C. for 2 to 6 hours depending on the composition.
- the obtained calcined powder was pulverized to 0.6 to 1.5; ⁇ ⁇ by wet pulverization, and then the pulverized powder was dried.
- the obtained granulated powder was molded to a molding density of 2 to 4 g / cm 3 with a uniaxial press machine.
- the obtained molded body was debindered at 300 ° C to 700 ° C and then sintered at 1500 ° C to 1800 ° C for 10 to 50 hours in an atmosphere with an oxygen concentration of 50 to 100%. Obtained.
- the obtained sintered body was processed into ⁇ 10 mm x 4 to 9 mm to obtain a test piece.
- the obtained specimen was measured for relative permittivity, Qf value, and ⁇ ⁇ "value by H & C method using a network analyzer. The measurement results are shown in Table 1.
- Test pieces ⁇ .1 to 43 are examples according to the present invention, and ⁇ .44 to 56 are comparative examples.
- ⁇ .44 is the same as Example No.l, and when y (Ln), z (Ga), m (Ca) is not included, No.45 ⁇ 49 is Z ( When no Ga) is included, No. 50 does not contain m (Ca) in the Example No. 1 composition, No. 51 and 52 show No. 51 when X is out of the range in the Example No. 1 composition.
- Example No.l composition does not contain y (Ln), x is out of range, No.54 is Example No.l composition y (Ln) is out of range, No .55 is Example No.l composition when V and z (Ga) are out of range, No.56 is Example No.l composition and m (Ca) is out of range It is a comparative example showing a certain case.
- the test piece according to the present invention has a Qf value in the vicinity of a relative dielectric constant of 39 of 57,000 to 88,000, and a ⁇ f value of -8 ppm / ° C to 6 ppm / ° C. It is apparent that the range can be controlled within the above range by selecting the composition.
- Fig. 1 shows the results of EPMA analysis of test piece No. 1 in Example 1, and Fig. 2 to Fig. 6 show schematic diagrams thereof.
- Fig. 1 Upper left is BEI (composition image, schematic diagram is shown in Fig. 2), upper middle is A1 characteristic X-ray image (Fig. 3 is schematic diagram), upper right is Ga characteristic X-ray image (Fig. 4)
- the middle left is a characteristic X-ray image of Ti (schematic diagram is shown in Fig. 5)
- the middle middle is a characteristic X-ray image of La (schematic diagram is shown in Fig. 6)
- the middle right is Sr.
- Characteristic X-ray image, lower left is a characteristic X-ray image of Ca.
- the part that appears white is the main phase
- the gray part is the thick black part in the schematic diagram
- the part surrounded by the line and the black line is the grain boundary.
- Characteristic of A1 and Ga In the X-ray image, the same part as the grain boundary part in the composition image (inside the line frame in the schematic diagrams of FIGS. 3 and 4) is white. This indicates that A1 and Ga exist at the grain boundaries.
- the characteristic X-ray images of Ti and La the same part as the grain boundary part in the composition image (in the line frame in the schematic diagrams of FIGS. 5 and 6) is black. This indicates that Ti and La do not exist at the grain boundaries.
- the grain boundary has (1) a solid solution of A ⁇ Ga-Sr oxide, (2) a solid solution of A ⁇ Ga oxide and Sr oxide, and (3) A ⁇ Ga-Sr oxide. It can be determined that Al, Ga, and Sr are present in any form of solid solution of matter and solid solution of A ⁇ Ga-based oxide and Sr oxide.
- Fig. 7 shows the X-ray diffraction results of the test pieces with various amounts of Ca substitution.
- m 0 (test piece No. 43)
- m 0.05 (test piece No. 1)
- m 0.10 (Specimen No. 2).
- m 0.20 (test specimen No. 4)
- m 0.30 (test specimen No. 6).
- Each specimen was calcined at 1300 ° C for 4 hours.
- FIG. 1 is a composition image and characteristic X-ray image showing the results of EPMA analysis of the dielectric ceramic composition for electronic devices of the present invention.
- FIG. 2 is a schematic diagram showing the BEI (composition image) of FIG.
- FIG. 3 is a schematic diagram showing a characteristic X-ray image of A1 in FIG.
- FIG. 4 is a schematic diagram showing a characteristic X-ray image of Ga in FIG. 1.
- FIG. 5 is a schematic diagram showing a characteristic X-ray image of Ti in FIG. 1.
- FIG. 6 is a schematic diagram showing a characteristic X-ray image of La in FIG. 1.
- FIG. 7 is a graph showing the X-ray diffraction results of the dielectric ceramic composition for electronic devices of the present invention.
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Application Number | Priority Date | Filing Date | Title |
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PCT/JP2005/011651 WO2006137153A1 (ja) | 2005-06-24 | 2005-06-24 | 電子デバイス用誘電体磁器組成物 |
KR1020077029937A KR101118425B1 (ko) | 2005-06-24 | 2005-06-24 | 전자디바이스용 유전체 자기 조성물 |
EP05752963A EP1900707A4 (en) | 2005-06-24 | 2005-06-24 | DIELECTRIC CERAMIC COMPOSITION FOR ELECTRONIC COMPONENT |
US11/993,700 US7648935B2 (en) | 2005-06-24 | 2005-06-24 | Dielectric porcelain composition for use in electronic devices |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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PCT/JP2005/011651 WO2006137153A1 (ja) | 2005-06-24 | 2005-06-24 | 電子デバイス用誘電体磁器組成物 |
Publications (1)
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WO2006137153A1 true WO2006137153A1 (ja) | 2006-12-28 |
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PCT/JP2005/011651 WO2006137153A1 (ja) | 2005-06-24 | 2005-06-24 | 電子デバイス用誘電体磁器組成物 |
Country Status (4)
Country | Link |
---|---|
US (1) | US7648935B2 (ja) |
EP (1) | EP1900707A4 (ja) |
KR (1) | KR101118425B1 (ja) |
WO (1) | WO2006137153A1 (ja) |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2004091266A (ja) * | 2002-08-30 | 2004-03-25 | Daiken Kagaku Kogyo Kk | ガリウム添加形誘電体磁器組成物、誘電体共振器及びマイクロ波通信装置 |
RU2242442C1 (ru) * | 2003-04-17 | 2004-12-20 | Ненашева Елизавета Аркадьевна | Способ формирования состава твердых растворов для изделий высокочастотной и микроволновой техники (варианты) |
JP2005514298A (ja) * | 2000-10-30 | 2005-05-19 | 株式会社Neomax | マイクロ波用誘電体磁器組成物 |
JP2005194114A (ja) * | 2003-12-26 | 2005-07-21 | Neomax Co Ltd | 電子デバイス用誘電体磁器組成物 |
Family Cites Families (7)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2625074B2 (ja) | 1992-06-24 | 1997-06-25 | 京セラ株式会社 | 誘電体磁器組成物および誘電体共振器 |
JP3559434B2 (ja) | 1997-09-30 | 2004-09-02 | 京セラ株式会社 | 誘電体磁器組成物の製造方法 |
JP3744660B2 (ja) | 1997-10-30 | 2006-02-15 | 京セラ株式会社 | 誘電体磁器組成物及びこれを用いた誘電体共振器 |
JP3974723B2 (ja) | 1998-01-14 | 2007-09-12 | 京セラ株式会社 | 誘電体磁器の製造方法 |
KR100415757B1 (ko) | 1999-01-14 | 2004-01-31 | 교오세라 가부시키가이샤 | 유전체 자기(誘電體磁器)조성물, 유전체 자기의 제조방법 및 유전체 공진기(共振器) |
JP2003034573A (ja) * | 2000-11-20 | 2003-02-07 | Kyocera Corp | 誘電体磁器及びこれを用いた誘電体共振器 |
GB2429011B (en) * | 2005-08-10 | 2007-05-30 | Filtronic Comtek | Microwave Dielectric Ceramic |
-
2005
- 2005-06-24 EP EP05752963A patent/EP1900707A4/en not_active Withdrawn
- 2005-06-24 US US11/993,700 patent/US7648935B2/en not_active Expired - Fee Related
- 2005-06-24 KR KR1020077029937A patent/KR101118425B1/ko not_active IP Right Cessation
- 2005-06-24 WO PCT/JP2005/011651 patent/WO2006137153A1/ja not_active Application Discontinuation
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2005514298A (ja) * | 2000-10-30 | 2005-05-19 | 株式会社Neomax | マイクロ波用誘電体磁器組成物 |
JP2004091266A (ja) * | 2002-08-30 | 2004-03-25 | Daiken Kagaku Kogyo Kk | ガリウム添加形誘電体磁器組成物、誘電体共振器及びマイクロ波通信装置 |
RU2242442C1 (ru) * | 2003-04-17 | 2004-12-20 | Ненашева Елизавета Аркадьевна | Способ формирования состава твердых растворов для изделий высокочастотной и микроволновой техники (варианты) |
JP2005194114A (ja) * | 2003-12-26 | 2005-07-21 | Neomax Co Ltd | 電子デバイス用誘電体磁器組成物 |
Also Published As
Publication number | Publication date |
---|---|
KR20080039343A (ko) | 2008-05-07 |
EP1900707A4 (en) | 2011-02-23 |
US20080227622A1 (en) | 2008-09-18 |
KR101118425B1 (ko) | 2012-03-06 |
EP1900707A1 (en) | 2008-03-19 |
US7648935B2 (en) | 2010-01-19 |
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