WO2022054337A1 - 低温共焼成基板用組成物 - Google Patents

低温共焼成基板用組成物 Download PDF

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Publication number
WO2022054337A1
WO2022054337A1 PCT/JP2021/018539 JP2021018539W WO2022054337A1 WO 2022054337 A1 WO2022054337 A1 WO 2022054337A1 JP 2021018539 W JP2021018539 W JP 2021018539W WO 2022054337 A1 WO2022054337 A1 WO 2022054337A1
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Prior art keywords
mass
powder
firing
particle size
sio
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Ceased
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PCT/JP2021/018539
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English (en)
French (fr)
Japanese (ja)
Inventor
恵斗 佐藤
延仁 武島
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Okamoto Glass Co Ltd
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Okamoto Glass Co Ltd
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Application filed by Okamoto Glass Co Ltd filed Critical Okamoto Glass Co Ltd
Priority to US17/802,528 priority Critical patent/US12466761B2/en
Priority to KR1020227034349A priority patent/KR102633693B1/ko
Priority to CN202180018640.3A priority patent/CN115210195B/zh
Priority to JP2022547393A priority patent/JP7323879B2/ja
Priority to EP21866298.9A priority patent/EP4108646B1/en
Publication of WO2022054337A1 publication Critical patent/WO2022054337A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C03C10/0054—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing PbO, SnO2, B2O3
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Definitions

  • the present invention relates to a composition for a low temperature co-fired ceramic (LTCC) substrate mainly used for a small integrated module for wireless communication.
  • LTCC low temperature co-fired ceramic
  • Front-End refers to elements that directly communicate with the outside, such as display to users, reception of operations, input / output to and from other systems, and Front-End Modules is a communication standard for mobile phones. It refers to an ultra-compact integrated module that integrates various functional components used in wireless front-end circuits such as LTE, Wi-Fi, Bluetooth, and GPS.
  • the LTCC substrate is a kind of ceramics used for electronic materials, and is so called because the ceramic carrier structure, the conductive resistance, and the dielectric material are simultaneously fired in a kiln at a temperature of less than 1000 ° C. It is used as an electronic circuit board by combining a plurality of capacitors and resistors incorporated in one layer.
  • millimeter waves are known to have extremely high straightness and a large amount of information transmission, but the material characteristics of the LTCC substrate that make use of this characteristic are that the signal attenuation of the circuit is small and that high-speed signal propagation is possible. It is required to be. Against this background, the required characteristics of the substrate material used for the LTCC substrate are increasing.
  • the signal attenuation in the high frequency region consists of the sum of the conductor loss and the dielectric loss, but in the region exceeding 1 GHz, the signal attenuation due to the dielectric loss of the LTCC substrate material becomes dominant.
  • the signal propagation velocity V has a relationship of V ⁇ k ⁇ 1/2 when the dielectric constant of the material is k. Therefore, in order to make the best use of the characteristics of millimeter-wave communication (realize high-speed signal transmission), a material having a high Q value (High Q) and a low dielectric constant (Low k) is required.
  • the network structure constituting the glass is deformed by an electric field, and deformation loss (Deformation Loss) is caused by the occurrence of bipolar orientation.
  • the vibration loss (Vibration Loss) generated by the lattice constituting the material resonating with the applied frequency occupies a large proportion. These losses generally increase in proportion to the frequency. It is known that the deformation and vibration loss of crystals, which have a strong structure and are less likely to be deformed or vibrated, are smaller than those of glass, which is amorphous.
  • the former method is disclosed in, for example, Cited Document 1.
  • an alkali borosilicate glass powder having a low relative permittivity and a low dielectric loss containing Li 2 O, Na 2 O, and K 2 O in a predetermined molar ratio is disclosed, and the glass powder and 20 to 50% by mass are disclosed.
  • a glass-ceramic dielectric material made of the above-mentioned ceramic filler powder and a sintered body obtained by sintering the same are disclosed.
  • the alkaline borosilicate glass is preferably an amorphous glass in which crystals do not precipitate even when sintered, because the softening fluidity at the time of sintering is good and a dense sintered body can be easily obtained. It is supposed to be.
  • Cited Document 2 The latter method seems to be disclosed in Cited Document 2.
  • CaO-B 2 O 3 -SiO having a composition of about 18 to 32% by weight of B 2 O 3 , about 42 to 47% by weight of CaO, and about 28 to 40% by weight of SiO 2 .
  • Crystallized glass from system 2 and non-crystalline glass having a composition of at least about 60% by weight SiO 2 , about 10 to 35% by weight B 2 O 3 , and about 6% by weight of alkali metal oxide. It is stated that it provides non-crystalline glass / glass ceramic, including.
  • Reference 3 discloses a sintered dielectric material containing a solid portion containing silica powder and a multi-component borosilicate glass component before sintering, and is selected from the group containing silicate stone, calcium borate, and the like.
  • a sintered dielectric material further comprising one crystalline compound is disclosed.
  • the object of the inventions disclosed in these references is that they can be fired at a low temperature of 1100 ° C. or 1000 ° C. or lower, and have a low relative permittivity k and a high Q value (low dielectric loss tangent) in a high frequency region of 1 GHz or higher. It is an object of the present invention to provide a composition for co-firing having tan ⁇ ).
  • compositions for an LTCC substrate As a composition for an LTCC substrate, as described in the background art, a composition having a low relative permittivity k and a high Q value has been searched for.
  • another important characteristic of the LTCC substrate is that it does not react with silver (Ag), which is an electrode material, during low-temperature co-fired, silver does not migrate, and the LTCC substrate does not warp. ..
  • Cited Document 3 when only the glass component was fired without adding silica powder, it had a high Q value and a low k value, but the movement of silver was large, and it was co-fired with a silver conductor in LTCC applications.
  • the addition of silica powder to the glass component could also allow for the ability to regulate shrinkage of the dielectric material and control the movement of silver in the dielectric material during firing, as it is believed to cause problems. Although it is described, its composition and effect have not been clarified.
  • the present invention is a composition for a low-temperature co-firing substrate before co-firing.
  • A Glass powder having 83 to 91% by mass of CaO-B 2O 3 -SiO 2 as a basic composition
  • B 7.5 to 14% by mass of SiO 2 powder
  • C 1.5 to 3% by mass
  • the glass powder (A) has a particle size D 50 of 2.0 to 3.0 ⁇ m, CaO having a composition of 40.0 to 45.0% by mass, and B 2 having a composition of 9.0 to 20.0% by mass.
  • the SiO 2 powder (B) is a filler and comprises any of the following combinations (1) to (3).
  • the ⁇ -wallastonite (CaSiO 3 ) powder (C) is a filler having a particle size D 50 of 2.0 to 3.0 ⁇ m.
  • Relative permittivity k is 6.0 or less at 5 GHz
  • Q value (1 / tan ⁇ : reciprocal of dielectric loss tangent) is 500 or more
  • reflectance R 420 at wavelength 420 nm and reflectance R at wavelength 800 nm are provided.
  • a composition for a low temperature co-firing substrate characterized in that the ratio R 420 / R 800 (percentage) of 800 is 85% or more.
  • the composition for a low-temperature co-firing substrate before co-firing of the present invention is a glass powder having (A) 83 to 91% by mass of CaO-B 2 O 3 -SiO 2 as an essential component, (B) 7. .5 to 14% by mass of SiO 2 powder, and (C) 1.5 to 3% by mass of ⁇ -wollastonite (CaSiO 3 ) powder, but other components such as ZrO 2 in less than 3% by mass. It may contain an oxide having high chemical stability.
  • the concentration of the glass powder needs to be 83 to 91% by mass. If it exceeds 91% by mass, the relative permittivity k exceeds 6.0 and becomes large. On the other hand, when it is less than 83% by mass, the amount of SiO 2 powder added becomes large, the sinterability due to co-firing deteriorates, and as a result, the dielectric loss tang tan ⁇ becomes large and the Q value falls below 500.
  • the composition of the glass powder (A) contains 40.0 to 45.0% by mass of CaO, 9.0 to 20.0% by mass of B 2 O 3 , and 40.0 to 46.0% by mass of SiO 2 . However, it may contain less than 2% by mass of an oxide having high chemical stability such as Al 2O 3 , ZrO 2 , and MgO.
  • the particle size D 50 of the glass powder is 2.0 to 3.0 ⁇ m. With the miniaturization of ceramic chip parts, the sheet thickness of the LTCC substrate has been reduced to 50 ⁇ m or less, and the thickness of the co-fired conductive paste is mainly 10 ⁇ m or less.
  • the glass code number OG305 has a CaO concentration of slightly less than 40% by mass, but there is a problem that the tan ⁇ is close to the allowable limit and the crystallization temperature Tc is slightly high (890 ° C.).
  • OG307 having a SiO 2 concentration lower than 40% by mass and a CaO concentration higher than 45% by mass tan ⁇ and crystallization temperature are not a problem, but a glass layer is formed on the surface during firing and a firing setter (used for firing). There will be manufacturing problems such as causing fusion to the shelf board / ceramic fireproof material in the form of a floor board.
  • OG310 In OG310 , OG311, OG315 and OG320 having a B2O3 concentration of less than 9.0% by mass, the degree of crystallinity is high, the shrinkage associated with crystallization is large, and the residual glass phase is reduced, and the shrinkage of the silver electrode is combined with the shrinkage of the silver electrode. The deviation from the behavior becomes large, and a large warp occurs in the LTCC substrate.
  • OG322 which has a CaO concentration lower than 40% by mass, the relative permittivity is as small as 4.5, but it is the sinterability that the relative permittivity is low despite the precipitation of ⁇ -wollastonite. Is not good (there are many holes). This point is also confirmed by electron micrographs.
  • ⁇ -wollastonite powder which is a filler, is used as a crystallization agent, and ⁇ from CaO-B 2 O 3 -SiO 2 glass having the composition of a, b, c or d selected in the previous paragraph.
  • -Wollastonite crystals are precipitated as the main crystal phase.
  • some CaB 2 O 4 crystals may precipitate as a by-crystal phase.
  • the reason why ⁇ -wollastonite is preferable to ⁇ -wallastonite is that the relative permittivity k value is low.
  • the amount of ⁇ -wollastonite powder added for the ⁇ -wollastonite powder to act as a crystal nucleus is 1.5 to 3.0% by mass. If it is less than this, the crystallization effect will be small, and if it is more than this, the effect will not change. Further, it is appropriate that the particle size D 50 of the ⁇ -wollastonite powder is 2.0 to 3.0 ⁇ m, which is about the same as the particle size D 50 of the glass powder A.
  • the SiO 2 powder as a filler is used to reduce the relative permittivity k. Further, some SiO 2 powder is incorporated into the B 2 O 3 rich residual glass phase remaining after crystal precipitation, and some SiO 2 powder surrounds the B 2 O 3 rich residual glass phase to form a silver electrode. It is possible to suppress the interaction with and to suppress the deterioration of the electrode due to the migration of silver. Then, it was found that it is essential to use two or more kinds of Nanometer-sized SiO 2 powders having different particle size ranges in order to exert the function of such SiO 2 powders.
  • the amount of SiO 2 powder to be added needs to be 7.5 to 14% by mass.
  • the relative permittivity k becomes more than 6.0, and the yellowing of the silver electrode described below becomes remarkable, and R 420 / R 800 becomes less than 85%.
  • the sinterability in co-firing deteriorates and tan ⁇ increases (Q value is less than 500).
  • the particle size of the SiO 2 powder is preferably 10 to 30% by mass of a powder having a particle size D 50 of 10 to 100 nm and 70 to 90% by mass of a powder having a particle size D 50 of 400 to 3000 nm.
  • the powder having a particle size D 50 of 100 to 400 nm is 60% by mass or more and the particle size D 50 is less than 40% by mass of the powder having a particle size D 50 of 400 to 3000 nm.
  • the powder having a particle size D 50 of 10 to 100 nm is 4 to 20% by mass
  • the powder having a particle size D 50 is 60 to 95% by mass
  • the powder having a particle size D 50 is 400 to 3000 nm is 0 to 36.
  • Those composed of% by mass are preferable. When it is out of these ranges, it becomes difficult to suppress the interaction with the silver electrode while maintaining the low k value and the high Q value, and to suppress the deterioration of the electrode due to the migration of silver.
  • the interaction between the silver electrode and the residual glass phase and the migration of silver to the residual glass phase can be evaluated by measuring the reflectance of the LTCC substrate after co-firing. This is because the silver atoms transferred to the residual glass phase are colloidal particles, and selective absorption peculiar to silver colloid occurs at a wavelength of around 420 nm and is observed as yellowing. Therefore, by measuring the ratio R 420 / R 800 of the reflectance R 800 at a wavelength of 800 nm, which is not affected by the silver colloidal particles, and the reflectance R 420 at 420 nm, the reflectance of which is reduced by absorption by the silver colloidal particles, yellow. From the degree of change, the amount of movement of silver atoms to the residual glass phase can be relatively evaluated.
  • the LTCC substrate has a relative permittivity k of 6.0 or less at 2.5 GHz, a Q value (1 / tan ⁇ : inverse of dielectric loss tangent) of 500 or more, and a reflectance of R 420 at a wavelength of 420 nm.
  • the ratio R 420 / R 800 (percentage) of the reflectance R 800 at a wavelength of 800 nm can be 85% or more.
  • the ⁇ -wollastonite powder promotes the precipitation of ⁇ -wollastonite crystals in the CaO-B 2 O 3 -SiO 2 system glass, and the crystal precipitates. Since the SiO 2 powder is taken into the later B 2 O 3 rich residual glass phase, and the SiO 2 powder surrounds the residual glass phase, the B 2 O 3 rich residual glass phase and the silver electrode are formed. It is possible to suppress the interaction with and the migration of silver to the B 2 O 3 rich residual glass phase. As a result, it is possible to obtain an LTCC substrate without yellowing of the silver electrode (without deterioration of the silver electrode) while maintaining a low k value and a high Q value.
  • It shows the temperature profile at the time of firing the composition for a low temperature co-firing substrate of this invention. It is a schematic diagram which shows the sample to measure R 420 / R 800 and the measurement position. The reflectance profiles obtained for R 420 / R 800 of Example 12 and Comparative Example 19 of the present invention are shown. It is an example (Example 12) of the X-ray diffraction profile after firing of the composition for a low temperature co-firing substrate of this invention. It is an electron micrograph showing the surface state after co-firing (the effect of adding ⁇ -wollastonite powder and the effect of adding two or more kinds of nanoSiO 2 powders).
  • a glass composition screening was performed to determine a suitable glass composition for use in the present invention.
  • a green sheet was prepared from the glass powder (without adding SiO 2 powder and ⁇ -wollastonite) by the same method as shown below, and fired at the temperature profile shown in FIG. Obtained a substrate.
  • the relative permittivity k and tan ⁇ (Q value) of the substrate after firing were measured. The results are summarized in Table 1. Then, for the reason described in paragraph [0017], the glass composition symbols a, b, c and d were selected as the glass powder A.
  • the glass that has passed through the above sieve is pulverized and classified by an ultrafine powder pulverizer with a built-in medium stirring type classifier whose pulverization conditions are adjusted so that the particle size D 50 is 2.0 to 3.0 ⁇ m, and each of them is shown in Table 3.
  • a glass powder A having a particle size D 50 described in 1 was obtained.
  • the particle size D 50 was measured by a laser diffraction method (manufactured by HORIBA, Ltd./LA-950V2) using a particle size distribution measuring machine. The measurement results are shown in Table 3.
  • SiO 2 powder B (Preparation of SiO 2 powder B) Regarding SiO 2 powder B, AEROSIL® R805 manufactured by Nippon Aerosil Co., Ltd. as a powder of 10 to 100 nm, SO-C1 manufactured by Admatex Co., Ltd. as a powder of 100 to 400 nm, and a powder of 400 to 3000 nm. SO-C2 manufactured by Admatex Co., Ltd. or Fuselex / X manufactured by Tatsumori Co., Ltd. was used. Table 3 shows the mixing ratio of SiO 2 powder having each particle size.
  • ⁇ -Wollastonite powder C (Preparation of ⁇ -Wollastonite powder C) Commercially available ⁇ -wollastonite crystal powder is pulverized with a dry ball mill while adjusting the pulverization time so that the particle size D 50 is 2.0 to 3.0 ⁇ m, and is classified using a sieve with an opening of 100 ⁇ m. A ⁇ -wollastonite powder having a particle size D 50 of 2.4 ⁇ m was obtained.
  • the obtained green sheet was laminated with 40 layers using a hot water laminator / WL28-45-200 manufactured by Nikkiso Co., Ltd. under a water temperature of 70 ° C. and a pressure of 20.7 MPa for 10 minutes under hydrostatic pressure, and is shown in FIG.
  • a low temperature firing substrate was obtained by firing according to a temperature program.
  • the heating rate up to 450 ° C. was 1 ° C./min
  • the debinder treatment was performed by keeping the temperature at 450 ° C. for 2 hours.
  • the temperature was raised to 850 ° C. at 2 hrs, and the temperature was kept at 850 ° C. for 15 minutes to carry out the crystallization treatment.
  • a muffle furnace manufactured by Motoyama Co., Ltd. was used for firing, and about 100 L / min of air was introduced for firing.
  • the obtained low-temperature calcined substrate was processed into a shape of about 3 ⁇ 4 ⁇ 30 mm, and the relative permittivity k and the dielectric loss tangent (tan ⁇ ) were measured by a perturbation method cavity resonator method.
  • the dielectric property was measured using a relative permittivity / dielectric loss tangent measurement system (TMR-2A) manufactured by Keycom. The measurement results are shown in Table 3.
  • Example 12 no decrease in reflectance was observed at 420 nm, and R 420 / R 800 was 88.6%, whereas in Comparative Example 19, it became a silver colloid at 420 nm. The resulting decrease in reflectance was observed, and it was found that R 420 / R 800 decreased to 75.2%.
  • As the silver paste to be applied a silver paste manufactured by Noritake Co., Ltd. Limited was used.
  • the calcined low-temperature calcined substrate is crushed in an alumina magnetic mortar, and the crystal phase is identified from the peak position by measuring in the range of 15 to 35 degrees using an X-ray diffractometer / X'Pert PRO manufactured by Malvern Panasonic. rice field.
  • An example of the identification result (Example 12) is shown in FIG. From the identification results, ⁇ -wollastonite was detected as the main crystal phase, and CaB2O4 phase was detected as the subcrystal phase.
  • Table 3 shows a summary of the measurement results of the above examples.
  • the B 2 O 3 rich is maintained while maintaining the low k value and high Q value. It is possible to suppress the interaction between the residual glass phase and the silver electrode and the migration of silver to the B2O3 rich residual glass phase ( R 420 / R 800 is achieved at 85.0% or more). I understood.
  • Comparative example A comparative example is shown in Table 4.
  • the concentrations of the glass powder A, the SiO 2 powder B and the ⁇ -wollastonite powder C were out of the claims, and other than that, the particles of the SiO 2 powder B were obtained.
  • the content of the SiO 2 powder in the diameter range and the particle size range is outside the range of claims.
  • the Q value has not reached the target value of 500.
  • R 420 / R 800 was less than 85%, and remarkable yellowing occurred.
  • the SiO 2 powder having a fine particle size has a large specific surface area and attracts a large amount of the remaining B 2 O 3 rich glass phase, resulting in a silver B 2 O 3 rich glass phase.
  • migration is suppressed and R 420 / R 800 becomes large, if the amount of fine SiO 2 powder becomes too large, the structure after sintering becomes sparse and tan ⁇ increases (Comparative Example 9).
  • the SiO 2 powder having a coarse particle size has a relatively dense structure after sintering and can keep the tan ⁇ low, but when the amount of the coarse SiO 2 powder is large, the migration to the silver B 2 O 3 rich glass phase is performed.
  • the inhibitory effect is poor and R 420 / R 800 becomes small (Comparative Examples 7 and 14).
  • the relative permittivity is 6.0 or less and the tan ⁇ is 0.002 or less only when at least two or more of the three nanometer-sized SiO 2 powders are added at the ratios described in the claims. While maintaining (Q value of 500 or more), the interaction between the B 2 O 3 rich residual glass phase and the silver electrode and the migration of silver to the B 2 O 3 rich residual glass phase could be suppressed.

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