WO2018182180A1 - Matériau céramique diélectrique à haute fréquence à base de bmw et son procédé de fabrication - Google Patents

Matériau céramique diélectrique à haute fréquence à base de bmw et son procédé de fabrication Download PDF

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Publication number
WO2018182180A1
WO2018182180A1 PCT/KR2018/002315 KR2018002315W WO2018182180A1 WO 2018182180 A1 WO2018182180 A1 WO 2018182180A1 KR 2018002315 W KR2018002315 W KR 2018002315W WO 2018182180 A1 WO2018182180 A1 WO 2018182180A1
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WIPO (PCT)
Prior art keywords
ceramic material
high frequency
dielectric ceramic
metal element
frequency dielectric
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PCT/KR2018/002315
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English (en)
Korean (ko)
Inventor
윤상옥
김신
홍창배
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강릉원주대학교산학협력단
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Priority claimed from KR1020180020807A external-priority patent/KR102023398B1/ko
Application filed by 강릉원주대학교산학협력단 filed Critical 강릉원주대학교산학협력단
Priority to JP2020503679A priority Critical patent/JP6883142B2/ja
Priority to CN201880026647.8A priority patent/CN110603610B/zh
Priority to US16/499,862 priority patent/US11027985B2/en
Publication of WO2018182180A1 publication Critical patent/WO2018182180A1/fr

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/02—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances
    • H01B3/10—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances metallic oxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/02—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances
    • H01B3/12—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances ceramics

Definitions

  • the present invention relates to a dielectric ceramic material for resonators, filters, and oscillators used in a wireless communication system.
  • the present invention relates to a Ba (Mg 0.5 W 0.5 ) O 3 based high frequency dielectric ceramic material having an appropriate dielectric constant in a high frequency band and having a high quality factor. It is to provide a manufacturing method.
  • the present invention selected Ba (Mg 0.5 W 0.5 ) O 3 as a good material having high frequency dielectric properties.
  • a high frequency dielectric ceramic material composition having a high quality factor and stable temperature characteristics was prepared. If necessary, the +5 valent metal element can be added quantitatively to the tungsten (W) site.
  • microwave dielectric ceramics have been applied to mobile phones, wireless LAN (Local Area Network), GPS (Global Position Satellite), military radar system, Intelligent Transport System (ITS), etc. It is actively applied, and the dielectric ceramics for resonators, filters, and oscillators used in the system require an appropriate dielectric constant ( ⁇ r ), a high quality factor (Q ⁇ f), and a temperature coefficient close to zero ( ⁇ f ).
  • the high quality factor (Q ⁇ f) of Ba (Mg 0.5 W 0.5 ) O 3 is due to the 1: 1 regularization of B-site and generally improves the high frequency dielectric properties through the modification of the composition.
  • US Pat. No. 5,432,135 (1995.07.11.) Controls the composition ratio of the basic elements barium (Ba), magnesium (Mg) and tungsten (W), and as an additive yttrium oxide (Y 2 O 3 ), titanium oxide ( Disclosed is a high frequency dielectric ceramic material having improved dielectric properties using TiO 2 ), manganese oxide (MnO 2 ), and the like.
  • Japanese Patent Laid-Open No. 2000-044338 (2000.02.15.) Discloses Ba (Mg 0.5 W 0.5 ) O 3.
  • the dielectric properties are changed by substituting a part of strontium (Sr) in place of barium (Ba) and a certain amount of zinc (Zn), nickel (Ni) and cobalt (Co) in place of magnesium (Mg).
  • Sr strontium
  • Zn zinc
  • Ni nickel
  • Co cobalt
  • U.S. Patent No. 5,268,341 (1993.12.07.) Is characterized by improving the temperature coefficient ( ⁇ f ) of the resonant frequency by substituting tantalum (Ta) elements in place of tungsten (W).
  • Chinese Patent CN 102765938B (2014.04.02.) Discloses Ba (Mg 0.5 W 0.5 ) O 3
  • yttrium oxide (Y 2 O 3 ) or some rare earth oxides (RE 2 O 3 ) and zirconium oxide (ZrO 2 ) are substituted in place of magnesium (Mg), and manganese oxide (MnO 2 ) is added to 1
  • Mg yttrium oxide
  • RE 2 O 3 rare earth oxides
  • ZrO 2 zirconium oxide
  • Mg manganese oxide
  • MnO 2 manganese oxide
  • an alkali metal element such as sodium (Na) is placed in place of barium (Ba) in Ba (Mg 0.5 W 0.5 ) O 3 high frequency dielectric ceramic material.
  • + trivalent metal elements such as yttrium (Y) in place of magnesium (Mg) to partially replace and compensate for this, an excellent high frequency dielectric ceramic material composition having a high quality factor is disclosed.
  • an appropriate additive is selected in consideration of the substitution element size or valence associated with the crystal structure, and an appropriate amount of high-frequency dielectric ceramic material having a high quality factor and stable temperature characteristics is required. As can be developed, it has come to the present invention.
  • the present invention has been made to solve the above-mentioned problems, the present invention has a more appropriate dielectric constant, for example, to achieve a high quality factor of 100,000 GHz or more, preferably 150,000 GHz or more for removing noise and efficient transmission and reception It is an object of the present invention to provide a high frequency dielectric ceramic material capable of retaining the temperature coefficient of the resonant frequency improved to within ⁇ 10ppm / °C for the temperature stability of the transmission and reception frequency.
  • the present invention in the composition of (Ba 1-ab Ma a Mb b ) (Mg 0.5-c Mc c W 0.5 ) O 3 , Ma and Mb are alkali metals and alkaline earth metals, Mc is + 3 is a metal, a and c are each 0.01 to 0.1, and b is 0.09 to 0.25 to provide a MM-based high frequency dielectric ceramic material.
  • part of W is further substituted by Me, which is a +5 valent metal element, to form a composition of (Ba 1-ab Ma a Mb b ) (Mg 0.5-c Mc c W 0.5-e Me e ) O 3 , It is preferable that e is 0.01-0.05.
  • Ma is a + monovalent alkali metal element represented by Ma 2 O, and is preferably any one selected from Na, K, and Li.
  • the Mb is a + divalent alkaline earth metal element represented by MbO, and is preferably any one selected from Sr and Ca.
  • Mc is a + trivalent lanthanide metal element represented by Mc 2 O 3, and preferably any one selected from Sc, Y, Sm, Gd, Yb, and Dy or In boron group metal element.
  • Me is a + 5-valent vanadium group metal element represented by Me 2 O 5 , and is preferably any one selected from Nb and Ta.
  • the Ma and Mb is preferably all added for the purpose of high quality factor.
  • the Mb and Me is preferably added alone or all for the purpose of temperature characteristics of the resonance frequency.
  • the high frequency dielectric ceramic material has a more appropriate dielectric constant, and a high quality factor is realized.
  • the high frequency dielectric ceramic material according to the present invention has a stable temperature coefficient (for example, within ⁇ 10ppm / °C) it can be expected to exhibit good dielectric properties.
  • the high frequency dielectric ceramic material according to the present invention can be expected to have a high-quality high-frequency transmission and reception in the tens of GHz frequency band.
  • Figure 1 according to an embodiment of the present invention (Ba 1 -a- b Ma a Mb b) (Mg 0 .5- c YcW 0 .5- e Me e) O 3 series according to the Mb content of the high-frequency dielectric ceramic material, This graph shows the change in the temperature coefficient of the resonant frequency.
  • Figure 3 is according to the Me content of the (Ba 1 -a- b Ma a Sr b) according to an embodiment of the present invention (Mg 0 .5- c YcW .5- 0 e e Me) O 3 based high-frequency dielectric ceramic material,
  • This graph shows the change in the temperature coefficient of the resonant frequency.
  • an excellent ceramic dielectric requires the following characteristics.
  • an excellent ceramic dielectric resonator requires proper dielectric constant, high quality coefficient, and temperature coefficient of resonance frequency within ⁇ 10ppm / °C.
  • the temperature coefficient the more the value converges to 0, the better.
  • Ceramic material of the present invention was prepared by the following manufacturing method.
  • BaCO 3 purity 99.5% of SAKAI Chem. Ind. Co., Ltd., Na 2 CO 3 (purity: 99.5%) of Samjeon Pure Chemical Industries, Ltd., Japan High Purity Chemical Research Institute (Kojundo Chem. Lab. Co., Ltd) MgO (purity: 99%), Y 2 O 3 (purity: 99.9%), SrCO 3 (purity 99.9%), CaCO 3 (purity 99.5%), Ta 2 O 5 (purity: 99.9%), Nb 2 O 5 (purity: 99.9%) and WO 3 (purity: 99.9%) were used.
  • the mixed powder was placed in a metal mold having a diameter of 25 mm and uniaxially press-molded, and then calcined at 900 to 1100 ° C. for 10 hours.
  • the calcined molded body was again ball milled by the above mixing method, placed in an oven, and dried at 110 to 120 ° C. for 24 to 48 hours.
  • the dried powder was placed in a metal mold having a diameter of 15 mm and uniaxially press-molded at a pressure of 50 MPa, followed by sintering.
  • the sintering temperature and time were 1600-1700 ° C and 1 hour, and the temperature increase rate and the cooling rate up to 1200 ° C were 5 ° C / min.
  • the shrinkage ratio of the sintered body manufactured by the above method was measured and X-ray diffraction analysis (D / MAX-2500V / PC, Rigaku, Japan) was performed on the powder obtained by pulverizing the sintered body.
  • the quality coefficient (Q ⁇ f) and the temperature coefficient ( ⁇ f ) were measured by the cavity method, and the dielectric constant was measured by the network analyzer using the Hakki-Coleman method.
  • the temperature coefficient was used model name R3767CG (Advantest, Japan)
  • the quality coefficient and dielectric constant was used model name E5071C (Keysight, USA).
  • alkaline earth metal elements (group 2a) such as strontium (Sr)
  • + 5-valent metal elements such as tantalum (Ta)
  • the change of temperature characteristic of the resonant frequency was investigated.
  • alkaline earth metal elements (group 2a) such as strontium (Sr)
  • tantalum (Ta) was placed in the tungsten (W) site. Quantitative additions were arranged experimentally.
  • the quality factor is gradually reduced with strontium (Sr) content as shown in Figure 2 and can be seen to sharply lower at more than 0.25 mol, if not added depending on the content of sodium (Na) and yttrium (Y) It can be seen that the quality factor was greatly increased at 0.01 mol compared with that and then gradually decreased again. Therefore, sodium (Na) and yttrium (Y) should be added at least 0.01 mole, although not shown in the table, it is preferred to add up to 0.1 mole. The same is true for alkali metals other than sodium and yttrium (K, Li, etc.) and + trivalent metal elements (Al, Ga, Gd, Sm, etc.).
  • Table 2 replaces the barium (Ba) site with only alkaline earth metal elements and replaces the +5 valence vanadium metal element with the tungsten (W) site and compensates the charge.
  • + Trivalent metal elements Sc, Sm, Gd, Yb, Dy, etc.
  • the comparative example shows that only the alkali metal is substituted, and as shown in FIG. It can be seen that the number can be effectively controlled.
  • the result is similar even if yttrium (Y) is substituted for the trivalent lanthanide metal element Sc, Sm, Gd, Yb, Dy, or In, which is a boron metal element.
  • the temperature coefficient of the resonance frequency tends to increase linearly in accordance with the increase of strontium (Sr) and tantalum (Ta), and gradually increases when strontium (Sr) and tantalum (Ta) are added together.
  • strontium (Sr) and +5 valent vanadium group metal elements eg, Nb, Ta
  • the + 5-valent vanadium group metal element maintain the ratio (1-5 mol%) of 0.01-0.05 mol. In the case of less than 0.01 mole, the change in the temperature coefficient ⁇ f of the resonant frequency is too small, and when it exceeds 0.05 mole, the deterioration of the quality factor is not preferable.
  • the temperature coefficient of the resonant frequency is an important factor in the part design along with the quality factor.
  • +3 is added in place of magnesium (Mg).
  • Mg magnesium
  • the quantitative addition of metal elements and +5 in the place of tungsten (W) can be seen as a very efficient way to produce high frequency dielectric ceramic material compositions with high quality coefficients and stable temperature characteristics. .
  • the change of these properties can be regarded as a phenomenon associated with the change of crystal structure which is closely related to the ion radius and the substitution amount of the substitution element.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Control Of Motors That Do Not Use Commutators (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Inorganic Insulating Materials (AREA)

Abstract

La présente invention concerne un matériau céramique diélectrique pour un résonateur, un filtre et un oscillateur utilisé dans un système de communication sans fil. En particulier, l'invention concerne un matériau céramique diélectrique à haute fréquence à base de Ba(Mg0,5W0,5)O3 ayant une constante diélectrique appropriée et un facteur de qualité élevé dans une bande haute fréquence, et son procédé de fabrication. À cet effet, dans la présente invention, Ba(Mg0,5W0,5)O3 a été sélectionné en tant que matériau ayant de bonnes propriétés diélectriques à haute fréquence, le baryum (Ba) étant partiellement substitué par un métal alcalin ou un élément de métal alcalino-terreux, et pour compenser ce dernier, un élément métallique de valence +3 est ajouté quantitativement au site de magnésium (Mg). Ainsi, une composition de matériau céramique diélectrique à haute fréquence ayant un facteur de qualité élevé et une caractéristique de température stable est produite. Un élément métallique de valence +5 peut être ajouté quantitativement au tungstène (W) selon les besoins. Selon la présente invention telle que décrite ci-dessus, un matériau céramique diélectrique à haute fréquence est censé avoir une constante diélectrique plus appropriée, d'excellentes caractéristiques de température, et un facteur de qualité élevé.
PCT/KR2018/002315 2017-03-31 2018-02-26 Matériau céramique diélectrique à haute fréquence à base de bmw et son procédé de fabrication WO2018182180A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
JP2020503679A JP6883142B2 (ja) 2017-03-31 2018-02-26 Ｂｍｗ系高周波誘電体セラミックス素材及びその製造方法
CN201880026647.8A CN110603610B (zh) 2017-03-31 2018-02-26 Bmw类高频电介质陶瓷原材料及其制备方法
US16/499,862 US11027985B2 (en) 2017-03-31 2018-02-26 BMW-based high frequency dielectric ceramic material and method for manufacturing same

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KR20170041421 2017-03-31
KR10-2017-0041421 2017-03-31
KR10-2018-0020807 2018-02-21
KR1020180020807A KR102023398B1 (ko) 2017-03-31 2018-02-21 Ｂｍｗ계 고주파 유전체 세라믹 소재 및 그 제조방법

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5834405A (en) * 1990-05-18 1998-11-10 International Business Machines Corporation Superconducting multilayer ceramic substrate
EP0881199A1 (fr) * 1997-05-30 1998-12-02 Kyocera Corporation Céramiques diélectriques
JP2002087881A (ja) * 2000-09-18 2002-03-27 Kyocera Corp 誘電体磁器及びこれを用いた誘電体共振器
US20050122639A1 (en) * 2003-01-31 2005-06-09 Toshihiro Okamatsu Dielectric ceramic,process for producing the same and laminate ceramic capacitor
CN102765938A (zh) * 2012-07-10 2012-11-07 上海大学 一种新的高Q×f值微波介质陶瓷材料

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5834405A (en) * 1990-05-18 1998-11-10 International Business Machines Corporation Superconducting multilayer ceramic substrate
EP0881199A1 (fr) * 1997-05-30 1998-12-02 Kyocera Corporation Céramiques diélectriques
JP2002087881A (ja) * 2000-09-18 2002-03-27 Kyocera Corp 誘電体磁器及びこれを用いた誘電体共振器
US20050122639A1 (en) * 2003-01-31 2005-06-09 Toshihiro Okamatsu Dielectric ceramic,process for producing the same and laminate ceramic capacitor
CN102765938A (zh) * 2012-07-10 2012-11-07 上海大学 一种新的高Q×f值微波介质陶瓷材料

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