SI21615A - LOW SINTERABLE FERROELECTRIC CERAMICS BASED ON Li2O DOPED (Ba, Sr) TiO3 - Google Patents
LOW SINTERABLE FERROELECTRIC CERAMICS BASED ON Li2O DOPED (Ba, Sr) TiO3 Download PDFInfo
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Nizkosinterabilna feroelektrična keramika na osnovi (Ba,Sr)TiO3 dopiranega z Li2OLow -interactive ferroelectric ceramics based on (Ba, Sr) TiO 3 doped with Li 2 O
Predmet izuma je feroelektrična keramika na osnovi (Ba,Sr)TiO3, kateri z dodatkom L12O znižamo temperaturo sintranja na <920°C, kar omogoča sočasno sintranje s kovinskim srebrom.The subject of the invention is ferroelectric ceramics based on (Ba, Sr) TiO 3 , which with the addition of L12O lowers the sintering temperature to <920 ° C, which allows simultaneous sintering with metallic silver.
Nov razvojni trend, ki se pojavlja v mikrovalovni tehnologiji, omogoča integracijo pasivnih komponent (filtri, kondenzatorji, resonatorji) in znatno miniaturizacijo v primerjavi s konvencionalnimi dielektričnimi komponentami. To omogoča tehnologija nizkotemperatumo sočasno sintrane keramike - LTCC (ang. low temperature cofired ceramics). Bistvo tehnologije LTCC je integracija pasivnih komponent v večfunkcionalnih, tridimenzionalnih modulih. Ti moduli so sestavljeni iz posameznih keramičnih plasti z mikrovalovnim vezjem, ki je povezano v tridimenzionalno strukturo. Da se organsko vezivo odstrani, keramične plasti ter elektrodna kovina pa zgostijo, je potrebno takšno tridimenzionalno kompozitno strukturo termično obdelati. Sintranje poteka pri relativno nizki temperaturi, približno 900°C, ki je pogojena s karakteristikami elektrodne kovine v modulu. Sočasno sintranje kovinskih in keramičnih plasti je eden od najzahtevnejših postopkov pri proizvodnji modulov LTCC. Velike nepravilnosti v izdelku se lahko pojavijo zaradi neenake hitrosti krčenja kovine in keramike med sintranjem. Zaradi neenakega krčenja različnih plasti vzorca se lahko med samim procesom sintranja pojavijo različni defekti, kot so razpoke, gubanje, zvijanje, pokanje, delaminacija itd., ki povzročijo bistveno poslabšanje karakteristik modula oziroma celo izgubo funkcionalnosti.A new development trend emerging in microwave technology enables the integration of passive components (filters, capacitors, resonators) and significant miniaturization compared to conventional dielectric components. This is made possible by the low temperature co-sintered ceramics (LTCC) technology. The essence of LTCC technology is the integration of passive components in multifunctional, three-dimensional modules. These modules consist of individual ceramic layers with a microwave circuit that is connected into a three-dimensional structure. In order to remove the organic binder and thicken the ceramic layers and the electrode metal, such a three-dimensional composite structure must be thermally treated. The sintering takes place at a relatively low temperature, about 900 ° C, which is conditioned by the characteristics of the electrode metal in the module. Co-sintering of metal and ceramic layers is one of the most demanding processes in the production of LTCC modules. Large product imperfections can occur due to uneven metal shrinkage rates and ceramics during sintering. Due to unequal shrinkage of different layers of the sample, various defects can occur during the sintering process, such as cracks, wrinkling, twisting, cracking, delamination, etc., which cause a significant deterioration of the module's characteristics or even loss of functionality.
Zaradi specifične izdelave modula LTCC je potrebno izbirati zelo kompatibilne materiale, ki morajo poleg ustreznih dielektričnih lastnosti izpolnjevati še vrsto drugih zahtev povezanih s sočasnim sintranjem. Ena od teh zahtev je nizka temperatura sintranja. Tališča kovin so omejevalni faktor pri uporabi visokih temperatur sintranja. Keramika se torej mora sintrati pri temperaturi, ki je za 50°C do 100°C nižja od temperature tališča elektrode. Taljenje elektrod bi poškodovalo notranjo strukturo modula in s tem povzročilo izgubo funkcionalnosti. Izbor kovin je zelo omejen, ker so nizke mikrovalovne dielektrične izgube povezane z visoko prevodnostjo elektrodne kovine. Zaradi dobre prevodnosti in odpornosti proti oksidaciji se najpogosteje v tehnologiji LTCC uporablja srebro, ki ima tališče pri 961,9°C.Due to the specific construction of the LTCC, it is necessary to select very compatible materials which, in addition to the corresponding dielectric properties, must satisfy a number of other requirements related to simultaneous sintering. One of these requirements is the low sintering temperature. Metal melting points are a limiting factor when using high sintering temperatures. Ceramics must therefore be sintered at a temperature below 50 ° C to 100 ° C below the melting point of the electrode. Melting the electrodes would damage the internal structure of the module and thus cause a loss of functionality. The selection of metals is very limited because low microwave dielectric losses are associated with high conductivity of the electrode metal. Due to its good conductivity and resistance to oxidation, silver is most commonly used in LTCC technology, which has a melting point at 961.9 ° C.
Zaradi zahtevnosti termičnega procesiranja modulov LTCC je funkcionalnost keramičnih plasti v današnjih sistemih LTCC omejena na nizkodielektrične substratne materiale, pri čemer pa se intenzivno razvijajo tudi visokodielektrični kondenzatorski, feritni, polprevodni materiali itd., Vsi ti materiali bi naj bili s stališča termične obdelave in kemijske kompatibilnost združljivi z obstoječo tehnologijo LTCC.Due to the complexity of thermal processing of LTCC modules, the functionality of the ceramic layers in today's LTCC systems is limited to low-dielectric substrate materials, while high-dielectric capacitor, ferrite, semiconductor materials, etc. are being intensively developed, all of these materials being considered from the point of view of thermal treatment and chemical compatibility. compatible with existing LTCC technology.
Material, ki je predmet izuma, se uvršča v kategorijo novih materialov za tehnologijo LTCC ter za vse ostale tehnologije, kjer je potrebno sočasno sintranje keramike s srebrno elektrodo kot so na primer tehnologije za izdelavo nekaterih izvedb prilagodljivih dielektričnih resonatorjev [P.K. Petrov s sod., Elect. Lett., 37, 2001, str. 17], večplastnih kondenzatorjev [S.M. Rhim s sod., J. Am. Ceram. Soc., 83, 2000, str. 3009] in elementov s pozitivnim temperaturnim koeficienton upornosti [J.K. Lee s sod., J. Am. Ceram. Soc., 85, 2002, str. 1173]. Material temelji na trdni raztopini BaTiCb in SrTiCF s splošno formula (Bai_xSrx)TiO3 (v nadaljevanju BST). Je feroelektrik in se odlikuje po tem, da je dielektrična konstanta odvisna od prednapetosti oziroma, da je mogoče dielektrično konstanto uravnavati s prednapetostjo. Takšne materiale imenujemo električno prilagodljivi materiali. BST je zelo dobro raziskan električno prilagodljiv material, ki se lahko uporablja v obliki monolitnega keramičnega elementa ali pa v obliki debelih oziroma tankih filmov. Električne lastnosti trdne raztopine s sestavo (Bao 6Sro.4)Ti03 so: dielektrična konstanta -3400, dielektrične izgube tan5=10' m električna prilagodljivost Δε=16.4%. Lastnosti lahko z nizkimi koncentracijami dopantov (nr. Fe, Y, Ga, Mn) bistveno spremenimo. Posebej izrazito lahko znižamo dielektrične izgube celo pod tanb = 5TO’3 in zvečamo električno prilagodljivost na Δε=23.3% [S.B. Hemer s sod., Mater. Lett., 15, 1993, str 317],The inventive material is classified in the new materials category for LTCC technology and for all other technologies requiring the simultaneous sintering of ceramics with a silver electrode, such as technologies for making some versions of adaptive dielectric resonators [PK Petrov et al., Elect. Lett., 37, 2001, p. 17], multilayer capacitors [SM Rhim et al., J. Am. Ceram. Soc., 83, 2000, p. 3009] and elements with a positive temperature coefficient of resistance [JK Lee et al., J. Am. Ceram. Soc., 85, 2002, p. 1173]. The material is based on a solid solution of BaTiCb and SrTiCF with the general formula (Bai_ x Sr x ) TiO3 (hereinafter BST). It is a ferroelectric and is characterized by the fact that the dielectric constant depends on the prestress, or that the dielectric constant can be controlled by the voltage. Such materials are called electrically flexible materials. BST is a very well researched electrically adaptable material that can be used in the form of a monolithic ceramic element or in the form of thick or thin films. The electrical properties of the solid solution with the composition (Bao 6Sro.4) Ti03 are: dielectric constant -3400, dielectric losses tan5 = 10 'm electrical adaptability Δε = 16.4%. Properties can be significantly altered by low concentrations of dopants (eg Fe, Y, Ga, Mn). In particular, dielectric losses can be reduced even below tanb = 5TO ' 3 and increase the electrical adaptability to Δε = 23.3% [SB Hemer et al., Mater. Lett., 15, 1993, p. 317],
Osnovna težava, ki onemogoča uporabo BST v tehnologiji LTCC in vseh drugih napravah, ki zahtevajo sočasno sintranje keramike in srebra, je previsoka temperatura sintranja. Ta znaša za prah s sestavo (Bao.6Sro.4)Ti03 s povprečno velikostjo delcev pod 1 pm okoli 1350°C. V preteklosti so bile že izvedene nekatere študije, s katerimi seje poskušalo temperaturo sintranja BST ustrezno znižati. Z dodatkom B2O3 je mogoče temperaturo sintranja BST znižati na 1100 do 1150°C, pri čemer ostanejo dielektrične in feroelektrične lastnosti takšnega materiala podobne lastnostim nedopiranega BST [ S. M. Rhim, J. Amer. Ceram. Soc., 83, 2000, str. 1145], Z uporabo alumosilikatnih fluksov bistvenega znižanja temperature sintranja ni bilo mogoče doseči [H.F. Cheng s sod., J. Am. Ceram. Soc., 76, 1993, str. 827],The basic problem that prevents the use of BST in LTCC technology and all other devices requiring the simultaneous sintering of ceramics and silver is the sintering temperature being too high. This amounts to dust with a composition (Bao.6Sro.4) Ti03 with an average particle size below 1 pm of about 1350 ° C. In the past, some studies have already been conducted to try to lower the BST sintering temperature accordingly. With the addition of B2O3, the sintering temperature of BST can be lowered to 1100 to 1150 ° C, leaving the dielectric and ferroelectric properties of such a material similar to the properties of undoped BST [S. M. Rhim, J. Amer. Ceram. Soc., 83, 2000, p. 1145], a significant decrease in sintering temperature could not be achieved by using alumosilicate fluxes [H.F. Cheng et al., J. Am. Ceram. Soc., 76, 1993, p. 827],
Naloga in cilj izuma je izdelati BST prah, ki bi imel temperaturo sintranja <920°C ter bil pri teh pogojih kemijsko kompatibilen s kovinskim srebrom. To bi omogočilo sočasno sintranje BST prahu in srebrnih elektronskih elementov.It is an object of the invention to produce a BST powder having a sintering temperature <920 ° C and being chemically compatible with metallic silver under these conditions. This would allow for the simultaneous sintering of BST dust and silver electronic elements.
Po izumu je naloga rešena po neodvisnem patentnem zahtevku.According to the invention, the problem is solved according to an independent patent claim.
Izum bo opisan na osnovi izvedbenih primerov in slik, ki prikazujejo:The invention will be described on the basis of embodiments and illustrations showing:
Slika 1: Dinamičen dilatometerski posnetek zgoščevanja (Bao.6Sro.4)Ti03 prahu s povprečno velikostjo delcev 0.8 pm in dodatkom 1.5% L12O (hitrost segrevanja je 10°C/min),Figure 1: Dynamic dilatometer recording of the thickening (Bao.6Sro.4) Ti03 powder with an average particle size of 0.8 pm and the addition of 1.5% L12O (heating rate is 10 ° C / min),
Slika 2: Izotermni dilatometerski posnetek zgoščevanja (Bao.6Sro.4)Ti03 prahu s povprečno velikostjo delcev 0.8 pm in dodatkom 1.5% L12O,Figure 2: Isothermal dilatometer thickener (Bao.6Sro.4) Ti03 powder with an average particle size of 0.8 pm and the addition of 1.5% L12O,
Slika 3: Mikrostruktura keramike (Bao 6Sro.4)Ti03 z dodatkom 1.5% L12O, sintrane 2h na 900°C,Figure 3: Microstructure of ceramics (Bao 6Sro.4) Ti03 with the addition of 1.5% L12O, sintered for 2h at 900 ° C,
Slika 4: Frekvenčna in temperaturna odvisnost dielektričnosti keramike s sestavo (Bao.6Sro.4)Ti03 z dodatkom 0.5 ut.% L12O sintrane 2h pri 900°C.Figure 4: Frequency and temperature dependence of the dielectricity of ceramics with the composition (Bao.6Sro.4) Ti03 with the addition of 0.5 wt% L12O sintered for 2h at 900 ° C.
Po izumu se BST prahu, ki je lahko komercialen ali posebej sintetiziran, doda do 20 ut.% L12O v obliki oksida ali kateri koli drugi obliki, ki med termično obdelavo razpade in omogoči reakcijo Li+ ionov z BST (npr. L12CO3 ali CH3COOL1 - Li-acetat). Del BST tako reagira z Li+ in tvori Li-titanatno fazo, presežek BaO in SrO pa se kompenzira s tvorbo (Ba,Sr)-ortotitanatne faze. Opisana reakcija povzroči površinsko aktivacijo preostale BST faze, ki je posledica generacije površinskih strukturnih defektov, ter tvorbo tekoče faze med procesom sintranja. To pospeši zgoščevanje že pri zelo nizkih temperaturah (<920°C). Kljub prisotnosti tekoče faze zaradi zelo nizkih temperatur termične obdelave zrna BST ne rastejo vendar pa se njihova površinska struktura regenerira. Po končanem sintranju vsebuje BST keramika nizke koncentracije Li-titanatne in (Ba,Sr)-ortotitanatne faze ter matrično BST fazo, ki zagotavlja ustrezne dielektrične lastnosti ter tudi električno prilagodljivost.According to the invention, up to 20% by weight of L12O in the form of oxide or any other form which, during thermal treatment, decomposes and enables the reaction of Li + ions with BST (eg L12CO3 or CH3COOL1 - Li-acetate). Part of the BST thus reacts with Li + to form the Li-titanate phase, and the excess BaO and SrO is compensated by the formation of the (Ba, Sr) -ortotitanate phase. The reaction described results in the surface activation of the remaining BST phase resulting from the generation of surface structural defects and the formation of a liquid phase during the sintering process. This accelerates compaction even at very low temperatures (<920 ° C). Despite the presence of the liquid phase, due to the very low temperatures of thermal treatment, BST grains do not grow, but their surface structure regenerates. After sintering, BST contains ceramics with low concentrations of Li-titanate and (Ba, Sr) -ortotitanate phases, as well as a matrix BST phase, which provides adequate dielectric properties as well as electrical adaptability.
Izvedbeni primer 1:Example 1:
Predreagiranemu prahu s sestavo (Bao.6Sro.4)Ti03 dodamo 0.5 ut% Li2O v obliki 5% raztopine Li-acetata v ocetni kislini. Zmes homogeniziramo in kalciniramo lOh pri temperaturi 850°C. Kalcinat zmeljemo do povprečne velikosti delcev manjše od 1 pm ter tako pripravljen prah stisnemo v kolute, ki jih sintramo 2h pri 900°C. Dielektričnost tako pripravljene keramike pri 20°C in frekvenci 1MHz znaša 3470, dielektrične izgube tanb < 10-4, temperaturna in frekvenčna odvisnost dielektričnosti pa je prikazana na grafu po sliki 4. Električna prilagodljivost pri sobni temperaturi in prednapetosti 2kV/mm znaša 15.7%.To the pre-reacted powder with the composition (Bao.6Sro.4) Ti03 was added 0.5 wt% Li 2 O in the form of a 5% solution of acetic acid Li-acetate. The mixture was homogenized and calcined at 10OH at 850 ° C. The calcinate is ground to an average particle size of less than 1 pm and the powder thus prepared is compressed into sintered wheels for 2 hours at 900 ° C. The dielectricity of the ceramics thus prepared at 20 ° C and a frequency of 1MHz is 3470, the dielectric loss of tanb <10 -4 , and the temperature and frequency dependence of the dielectricity is shown in the graph in Figure 4. Electrical adaptability at room temperature and bias of 2kV / mm is 15.7%.
Izvedbeni primer 2:Example 2:
Predreagiranemu prahu s sestavo (Bao.6Sro.4)Ti03 dodamo 0.5 ut% Li2O v obliki polikristaliničnega L12CO3. Zmes homogeniziramo in kalciniramo lOh pri temperaturi 850°C. Kalcinat zmeljemo do povprečne velikosti delcev manjše od 1 pm ter tako pripravljen prah stisnemo v kolute, ki jih sintramo 2h pri 900°C. Dielektričnost tako pripravljene keramike pri 20°C in frekvenci 1MHz znaša 3456, dielektrične izgube tand<10-4, temperaturna in frekvenčna odvisnost dielektričnosti pa je enaka kot v izvedbenem primeru 1. Električna prilagodljivost pri sobni temperaturi in prednapetosti 2kV/mm znaša 15.7%Pre-reacted powder with the composition (Bao.6Sro.4) Ti03 was added 0.5 wt% Li 2 O in the form of polycrystalline L12CO3. The mixture was homogenized and calcined at 10OH at 850 ° C. The calcinate is ground to an average particle size of less than 1 pm and the powder thus prepared is compressed into sintered wheels for 2 hours at 900 ° C. The dielectricity of the thus prepared ceramics at 20 ° C and the frequency 1MHz is 3456, the dielectric loss tand <10 -4 , and the temperature and frequency dependence of the dielectricity is the same as in Execution Case 1. Electrical flexibility at room temperature and bias 2kV / mm is 15.7%
Izvedbeni primer 3:Example 3:
Predreagiranemu prahu s sestavo (Bao.6Sro.4)Ti03 dodamo 1.5 ut% Li2O v obliki 5% raztopine Li-acetata v ocetni kislini. Zmes homogeniziramo in kalciniramo lOh pri temperaturi 850°C. Kalcinat zmeljemo do povprečne velikosti delcev manjše od 1 pm ter tako pripravljen prah stisnemo v kolute, ki jih sintramo 2h pri 900°C. Dielektričnost tako pripravljene keramike pri 20°C in frekvenci 1MHz znaša 3260, dielektrične izgube tan5 = 7-10“4, temperaturna in frekvenčna odvisnost dielektričnosti pa se v nobeni karakteristiki bistveno ne razlikuje od odvisnosti prikazane v izvedbenem primeru 1. Električna prilagodljivost pri sobni temperaturi in prednapetosti 2kV/mm znaša 15.4%To the pre-reacted powder with the composition (Bao.6Sro.4) Ti03 was added 1.5 wt% Li 2 O in the form of a 5% solution of acetic acid Li-acetate. The mixture was homogenized and calcined at 10OH at 850 ° C. The calcinate is ground to an average particle size of less than 1 pm and the powder thus prepared is compressed into sintered wheels for 2 hours at 900 ° C. The dielectricity of the thus prepared ceramic at 20 ° C and the frequency 1MHz is 3260, the dielectric losses tan5 = 7-10 “ 4 , and the temperature and frequency dependence of the dielectricity is not significantly different from the one shown in embodiment 1. Electrical adaptability at room temperature and bias of 2kV / mm is 15.4%
Izvedbeni primer 4: Predreagiranemu prahu s sestavo (Bao gSroUTiCb dodamo 2.5 ut% Li2O v obliki 5% raztopine Li-acetata v ocetni kislini. Zmes homogeniziramo in kalciniramo lOh pri temperaturi 850°C. Kalcinat zmeljemo do povprečne velikosti delcev manjše od 1 pm ter tako pripravljen prah stisnemo v kolute, ki jih sintramo 2h pri 900°C. Dielektričnost tako pripravljene keramike pri 20°C in frekvenci 1MHz znaša 2730, dielektrične izgube tand = 1-10 3, temperaturna in frekvenčna odvisnost dielektričnosti pa se v nobeni karakteristiki bistveno ne razlikuje od odvisnosti prikazane v izvedbenem primeru 1. Električna prilagodljivost pri sobni temperaturi in prednapetosti 2kV/mm znaša 15.3%.Embodiment 4: Pre-reacted powder with composition (Bao gSroUTiCb was added 2.5 wt% Li 2 O in the form of a 5% solution of acetic acid Li-acetate. The mixture was homogenized and calcined lOh at a temperature of 850 ° C. The calcinate was ground to an average particle size of less than 1 pm and the powder thus prepared is compressed into sintered coils for 2h at 900 ° C. The dielectricity of the ceramics thus prepared at 20 ° C and 1MHz is 2730, and the dielectric losses tand = 1-10 3 , and the temperature and frequency dependence of the dielectricity in none does not differ significantly from the dependence shown in embodiment 1. Electrical flexibility at room temperature and bias of 2kV / mm is 15.3%.
Eksperimentalno smo preiskusili sestave, ki so vsebovale do 20 ut.% Li2O in ugotovili, da vse funkcionirajo tako, kot je v patentu opisano. Glede na dosežene dielektrične lastnosti so boljše keramike, ki vsebujejo do 10% ut. Li2O. Najboljše lastnosti izkazujejo keramike z največ 5 ut. % Li2O, katera je tudi opisana v izvedbenih primerih.Experiments were tested for compositions containing up to 20 wt% Li 2 O and found that they all function as described in the patent. Depending on the dielectric properties achieved, ceramics containing up to 10% by weight are better. Li 2 O. Ceramics with a maximum of 5 wt. % Li 2 O, which is also described in embodiments.
Nizkosinterabilna feroelektrična keramika na osnovi (Ba,Sr)TiO3 dopiranega z Li2O po izumu, ki je izdelana po standardnih metodah izdelave keramičnih elementov, z nalivanjem ali nalaganjem debelih slojev ali tvorbo tankoslojnih filmov, je značilna po tem, da je trdni raztopini (Bai.xSrx)TiO3 z 0>x>l dodanih do 20 ut.% Li2O v obliki oksida ali kateri koli drugi obliki, ki med termično obdelavo razpade in omogoči reakcijo Li+ ionov z BST.Low-interactivity ferroelectric ceramics based on (Ba, Sr) TiO3 doped with Li 2 O according to the invention, which is made according to standard methods of making ceramic elements, by pouring or depositing thick layers or forming thin films, characterized in that it is a solid solution ( Bai. X Sr x ) TiO3 with 0>x> l added up to 20 wt.% Li 2 O in the form of oxide or any other form that decomposes during thermal treatment and enables the reaction of Li + ions with BST.
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