WO2016136899A1 - 気密パッケージの製造方法 - Google Patents
気密パッケージの製造方法 Download PDFInfo
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- WO2016136899A1 WO2016136899A1 PCT/JP2016/055675 JP2016055675W WO2016136899A1 WO 2016136899 A1 WO2016136899 A1 WO 2016136899A1 JP 2016055675 W JP2016055675 W JP 2016055675W WO 2016136899 A1 WO2016136899 A1 WO 2016136899A1
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- WIPO (PCT)
- Prior art keywords
- sealing material
- material layer
- glass
- ceramic substrate
- glass substrate
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- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 5
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B18/00—Layered products essentially comprising ceramics, e.g. refractory products
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
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- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
- B81C1/00261—Processes for packaging MEMS devices
- B81C1/00269—Bonding of solid lids or wafers to the substrate
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- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/04—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with articles made from glass
- C04B37/045—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with articles made from glass characterised by the interlayer used
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- H01L23/12—Mountings, e.g. non-detachable insulating substrates
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- H01L23/15—Ceramic or glass substrates
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/01—Manufacture or treatment
- H10N30/02—Forming enclosures or casings
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
- C04B2237/59—Aspects relating to the structure of the interlayer
- C04B2237/592—Aspects relating to the structure of the interlayer whereby the interlayer is not continuous, e.g. not the whole surface of the smallest substrate is covered by the interlayer
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
- C04B2237/70—Forming laminates or joined articles comprising layers of a specific, unusual thickness
- C04B2237/708—Forming laminates or joined articles comprising layers of a specific, unusual thickness of one or more of the interlayers
-
- H—ELECTRICITY
- H03—ELECTRONIC CIRCUITRY
- H03H—IMPEDANCE NETWORKS, e.g. RESONANT CIRCUITS; RESONATORS
- H03H3/00—Apparatus or processes specially adapted for the manufacture of impedance networks, resonating circuits, resonators
- H03H3/007—Apparatus or processes specially adapted for the manufacture of impedance networks, resonating circuits, resonators for the manufacture of electromechanical resonators or networks
- H03H3/02—Apparatus or processes specially adapted for the manufacture of impedance networks, resonating circuits, resonators for the manufacture of electromechanical resonators or networks for the manufacture of piezoelectric or electrostrictive resonators or networks
Definitions
- the present invention relates to a method for manufacturing an airtight package by a sealing process using laser light (hereinafter referred to as laser sealing).
- ⁇ Efforts are being made to maintain the characteristics of the hermetic package and to extend its service life.
- a piezoelectric vibrator element is a sensitive element that easily deteriorates when exposed to oxygen or moisture in the surrounding environment. Therefore, it has been studied to incorporate the piezoelectric vibrator element into the piezoelectric vibrator package in an airtight state so as to maintain the characteristics of the piezoelectric vibrator package and extend its life.
- the glass substrate and the glass substrate are surrounded so as to surround the piezoelectric vibrator element in a state in which the glass substrate is opposed to the element base on which the piezoelectric vibrator element is arranged with a space therebetween.
- An airtight structure in which a gap between the element substrate and a sealing material layer is sealed has been studied.
- the element base ceramic, for example, alumina is generally used.
- the piezoelectric vibrator element has low heat resistance. Therefore, if the element substrate and the glass substrate are sealed by firing in the softening flow temperature range of the sealing material layer, the characteristics of the piezoelectric vibrator element may be thermally deteriorated.
- laser sealing has been studied as a sealing method for hermetic packages.
- only the portion to be sealed can be locally heated, so that it is possible to seal the element substrate and the glass substrate while preventing thermal degradation of elements having low heat resistance.
- laser sealing is a method in which the sealing material layer is locally heated to soften and flow the sealing material layer, so that the time required for sealing is short, and accordingly, the element substrate and the sealing material The time for the layer to react is also reduced. As a result, the reaction layer is not sufficiently formed at the interface between the element substrate and the sealing material layer, and the fixing strength between the element substrate and the sealing material layer is lowered.
- the present invention has been made in view of the above circumstances, and its technical problem is to provide a method capable of increasing the fixing strength between the element substrate and the sealing material layer without causing thermal degradation of the member accommodated therein.
- the idea is to increase the long-term reliability of the airtight package.
- the manufacturing method of the hermetic package of the present invention includes a step of preparing a ceramic base, forming a sealing material layer on the ceramic base, a glass substrate, and a sealing material on the ceramic base.
- Sealing material usually contains low melting point glass. This low-melting glass erodes the surface layer of the element substrate during laser sealing, and a reaction layer is generated.
- the element substrate is made of glass, a reaction layer is generated to some extent by laser sealing, and the fixing strength can be ensured.
- the element substrate is a ceramic, the low melting point glass hardly erodes the surface layer of the element substrate at the time of laser sealing, and the reaction layer is not sufficiently formed. That is, when the element substrate is glass, the reaction layer can be formed by laser sealing, but when the element substrate is ceramic, it is difficult to form the reaction layer by laser sealing.
- the ceramic substrate and the glass substrate are sealed by laser sealing.
- the fixing strength between the ceramic substrate and the sealing material layer can be increased, and the fixing strength between the glass substrate and the sealing material layer can be ensured.
- the sealing material layer is previously formed on the ceramic substrate by electric furnace firing or the like, the reaction layer can be sufficiently formed on the surface layer of the ceramic substrate.
- the method for manufacturing an airtight package of the present invention uses a ceramic base having a base and a frame provided on the base, and forms a sealing material layer on the top of the frame. In this way, it becomes easy to accommodate a member such as a piezoelectric vibrator element in the hermetic package.
- the top of the frame it is preferable to polish the top of the frame so that the surface roughness Ra of the top of the frame is less than 0.5 ⁇ m.
- a sealing material layer made of a sintered body of a sealing material on a ceramic substrate by applying and baking a sealing material paste.
- the method for manufacturing an airtight package of the present invention preferably uses a sealing material containing 55 to 95 volume% bismuth glass and 5 to 45 volume% refractory filler.
- Bismuth-based glass has better reactivity with ceramics than other types of glass. Thereby, the adhesion strength between the ceramic substrate and the sealing material layer can be increased.
- bismuth-based glass has a low melting point but high thermal stability (devitrification resistance). Thereby, it can soften and flow well at the time of laser sealing, and the accuracy of laser sealing can be increased.
- the “bismuth-based glass” refers to glass containing Bi 2 O 3 as a main component, and specifically refers to glass containing 50% by mass or more of Bi 2 O 3 in the glass composition.
- the average thickness of the sealing material layer is preferably less than 10 ⁇ m.
- the difference in thermal expansion coefficient between the ceramic substrate and the sealing material layer is less than 45 ⁇ 10 ⁇ 7 / ° C., and the thermal expansion coefficient between the sealing material layer and the glass substrate. Is preferably less than 45 ⁇ 10 ⁇ 7 / ° C.
- the hermetic package of the present invention is preferably manufactured by the above-described method for manufacturing an airtight package.
- the method for manufacturing an airtight package of the present invention includes a step of preparing a ceramic substrate and forming a sealing material layer on the ceramic substrate.
- a sealing material paste is applied on the ceramic substrate to form a sealing material film, and then the sealing material film is dried and the solvent is volatilized.
- a method of firing at a temperature higher than the softening point of the sealing material to incinerate the resin component in the sealing material paste (debinding treatment) and sinter (fixing) the sealing material is preferable. In this way, the sealing material layer can be easily formed and the fixing strength between the ceramic substrate and the sealing material layer can be increased.
- alumina, aluminum nitride, zirconia, mullite and the like are preferable from the viewpoint of material cost and sintering strength.
- a glass ceramic (hereinafter referred to as LTCC) obtained by sintering a green sheet laminate is also preferable as the ceramic substrate.
- Alumina is advantageous in terms of material costs.
- Aluminum nitride is advantageous from the viewpoint of heat dissipation.
- LTCC has the advantage that it is easy to produce a ceramic substrate having a frame portion.
- the thickness of the ceramic substrate is preferably 0.1 to 1.0 mm. Thereby, thickness reduction of an airtight package can be achieved.
- a ceramic base having a base and a frame provided on the base as the ceramic base, and form a sealing material layer on the top of the frame. In this way, it becomes easy to accommodate a member such as a piezoelectric vibrator element in the hermetic package.
- the surface roughness Ra of the top of the ceramic substrate is preferably less than 0.5 ⁇ m and not more than 0.2 ⁇ m, particularly 0.01 to 0.15 ⁇ m.
- the surface roughness RMS of the top of the ceramic substrate is preferably less than 1.0 ⁇ m, 0.5 ⁇ m or less, in particular 0.05 to 0.3 ⁇ m. In this way, the surface smoothness of the sealing material layer is improved, and the accuracy of laser sealing can be increased. As a result, it becomes possible to increase the sealing strength of the hermetic package.
- “Surface roughness Ra” and “surface roughness RMS” can be measured by, for example, a stylus type or non-contact type laser film thickness meter or surface roughness meter.
- the sealing material paste is preferably applied in a frame shape along the outer peripheral edge region of the ceramic substrate. In this way, the effective area that functions as a device can be expanded. Moreover, it becomes easy to accommodate a member such as a piezoelectric vibrator element in an airtight package.
- the frame portion is provided in a frame shape along the outer peripheral edge region of the ceramic substrate, and the sealing material paste is applied to the top of the frame portion.
- the effective area that functions as a device can be expanded.
- members such as a piezoelectric vibrator element, in the inside of a frame part.
- the sealing material paste is usually produced by kneading the sealing material and the vehicle with a three-roller or the like.
- a vehicle usually includes a resin and a solvent.
- the resin used for the vehicle acrylic ester (acrylic resin), ethyl cellulose, polyethylene glycol derivative, nitrocellulose, polymethylstyrene, polyethylene carbonate, polypropylene carbonate, methacrylic ester and the like can be used.
- Solvents used in vehicles include N, N′-dimethylformamide (DMF), ⁇ -terpineol, higher alcohol, ⁇ -butyllactone ( ⁇ -BL), tetralin, butyl carbitol acetate, ethyl acetate, isoamyl acetate, diethylene glycol monoethyl Ether, diethylene glycol monoethyl ether acetate, benzyl alcohol, toluene, 3-methoxy-3-methylbutanol, triethylene glycol monomethyl ether, triethylene glycol dimethyl ether, dipropylene glycol monomethyl ether, dipropylene glycol monobutyl ether, tripropylene glycol monomethyl ether , Tripropylene glycol monobutyl ether, propylene carbonate, dimethyl sulfoxide (DM O), N-methyl-2-pyrrolidone and the like can be used.
- DMF N′-dimethylformamide
- ⁇ -BL ⁇ -
- the sealing material for example, a composite powder of glass powder and refractory filler powder can be used.
- the glass powder various materials can be used, for example, bismuth glass, tin phosphate glass, vanadium glass, etc. can be used, from the viewpoint of thermal stability and depth of the reaction layer, Bismuth-based glass is preferred.
- the “tin phosphate glass” refers to a glass mainly composed of SnO and P 2 O 5 , and specifically includes SnO and P 2 O 5 in a total amount of 40% by mass or more in the glass composition.
- glass “Vanadium-based glass” refers to glass mainly composed of V 2 O 5 , and specifically refers to glass containing 25% by mass or more of V 2 O 5 in the total amount in the glass composition.
- the bismuth-based glass has a transition metal oxide content of 0.5% by mass or more (preferably 2 to 18% by mass, more preferably 3 to 15% by mass, still more preferably 4 to 12% by mass, particularly preferably glass composition). 5 to 10% by mass) is desirable. If it does in this way, light absorption characteristics can be improved, suppressing a fall of thermal stability.
- Bismuth-based glass contains, as a glass composition, Bi 2 O 3 67 to 90%, B 2 O 3 2 to 12%, ZnO 1 to 20%, CuO + Fe 2 O 3 0.5 to 18% by mass. It is preferable. The reason for limiting the content of each component as described above will be described below. In addition, in description of the containing range of each component,% display points out the mass%. “CuO + Fe 2 O 3 ” is the total amount of CuO and Fe 2 O 3 .
- Bi 2 O 3 is a main component for forming the reaction layer and a main component for lowering the softening point, and its content is preferably 67 to 87%, more preferably 70 to 85%, Particularly preferred is 72 to 83%.
- the content of Bi 2 O 3 is less than 67%, the reaction layer is difficult to be generated, and the softening point becomes too high, and the glass is difficult to soften even when irradiated with laser light.
- the content of Bi 2 O 3 is more than 90%, the glass becomes thermally unstable, and the glass tends to devitrify when melted, sintered (fixed), or sealed with laser.
- B 2 O 3 is a component that forms a glass network of bismuth-based glass, and its content is preferably 2 to 12%, more preferably 3 to 10%, still more preferably 4 to 10%, particularly preferably. 5-9%.
- the content of B 2 O 3 is less than 2%, the glass becomes thermally unstable, and the glass tends to be devitrified during melting, sintering (adhering), or laser sealing.
- the content of B 2 O 3 is more than 12%, the softening point becomes too high and the glass is difficult to soften even when irradiated with laser light.
- ZnO is a component that suppresses devitrification at the time of melting, sintering (adhering), or laser sealing, and lowers the coefficient of thermal expansion, and its content is preferably 1 to 20%, more preferably Is from 2 to 15%, more preferably from 3 to 11%, particularly preferably from 3 to 9%. If the ZnO content is less than 1%, it is difficult to obtain the above effect. On the other hand, if the ZnO content is more than 20%, the component balance in the glass composition is impaired, and conversely, the glass tends to devitrify.
- CuO + Fe 2 O 3 is a component having light absorption characteristics, and when irradiated with laser light having a predetermined emission center wavelength, CuO + Fe 2 O 3 is a component that easily absorbs the laser light and softens the glass.
- CuO + Fe 2 O 3 is a component that suppresses devitrification at the time of melting, sintering (adhering), or laser sealing.
- the content of CuO + Fe 2 O 3 is preferably 0.5 to 18%, more preferably 3 to 15%, still more preferably 3.5 to 15%, still more preferably 4 to 12%, and particularly preferably 5 to 10%. %.
- the CuO content is preferably 0 to 15%, 1 to 15%, 2 to 12%, 3 to 10%, particularly 4.5 to 10%.
- the content of Fe 2 O 3 is preferably 0 to 7%, 0.05 to 7%, 0.1 to 4%, especially 0.2 to 3%.
- Fe ions in iron oxide exist in the state of Fe 2+ or Fe 3+ .
- Fe ions in iron oxide are not limited to either Fe 2+ or Fe 3+ , and may be any. Therefore, in the present invention, even Fe 2+ is handled after being converted to Fe 2 O 3 .
- the ratio of Fe 2+ is preferably large.
- the ratio of Fe 2+ / Fe 3+ in iron oxide is 0. It is preferable to regulate to 0.03 or more (preferably 0.08 or more).
- SiO 2 is a component that improves water resistance.
- the content of SiO 2 is preferably 0 to 10%, 0 to 3%, in particular 0 to less than 1%. If the content of SiO 2 is more than 10%, the softening point becomes too high, and the glass is difficult to soften even when irradiated with laser light.
- Al 2 O 3 is a component that improves water resistance.
- the content of Al 2 O 3 is preferably 0 to 5%, 0 to 2%, in particular 0 to less than 0.5%.
- the softening point becomes too high and the glass is difficult to soften even when irradiated with laser light.
- MgO + CaO + SrO + BaO (total amount of MgO, CaO, SrO and BaO) is a component that suppresses devitrification at the time of melting, sintering (adhering), or laser sealing, and the content of MgO + CaO + SrO + BaO is preferably 0 to 15%, especially 0-10%. If the content of MgO + CaO + SrO + BaO is more than 15%, the softening point becomes too high, and the glass is difficult to soften even when irradiated with laser light.
- the contents of MgO, CaO and SrO are each preferably 0 to 5%, particularly preferably 0 to 2%.
- the content of BaO is preferably 0 to 10%, in particular 0 to 8%.
- CeO 2 , WO 3 , In 2 O 3 , Ga 2 O 3 and Sb 2 O 3 are components that suppress devitrification at the time of melting, sintering (adhering), or laser sealing.
- the content of each component is preferably 0 to 10%, 0 to 5%, 0 to 2%, particularly 0 to 1%. When the content of each component is more than 10%, the component balance in the glass composition is impaired, and conversely, the glass is easily devitrified. From the viewpoint of enhancing the thermal stability, it is preferable to add a small amount of Sb 2 O 3 , and specifically, it is preferable to add 0.05% or more of Sb 2 O 3 .
- the oxides of Li, Na, K and Cs are components that lower the softening point. However, since they have an action of promoting devitrification at the time of melting, the total amount is preferably regulated to less than 1%.
- P 2 O 5 is a component that suppresses devitrification at the time of melting. However, if the content of P 2 O 5 is more than 1%, the glass tends to undergo phase separation during melting.
- La 2 O 3, Y 2 O 3 and Gd 2 O 3 is a component to suppress phase separation during melting, when these total amount is more than 3%, the softening point becomes too high, the laser beam Even when irradiated, the glass becomes difficult to soften.
- NiO, V 2 O 5 , CoO, MoO 3 , TiO 2, and MnO 2 are components having light absorption characteristics. When irradiated with laser light having a predetermined emission center wavelength, the laser light is absorbed and glass is absorbed. It is a component that facilitates softening.
- the content of each component is preferably 0 to 7%, particularly 0 to 3%. If the content of each component is more than 7%, the glass tends to be devitrified during laser sealing.
- PbO is a component that lowers the softening point, but is a component that is concerned about environmental impact. Therefore, the content of PbO is preferably less than 0.1%.
- the refractory filler it is preferable to use one or more selected from cordierite, zircon, tin oxide, niobium oxide, zirconium phosphate ceramics, and willemite. These refractory fillers have a low thermal expansion coefficient, a high mechanical strength, and a good compatibility with bismuth glass. Of the above refractory fillers, cordierite is most preferred. Cordierite has a property that it is difficult to devitrify the bismuth glass even when the particle size is small, even when laser sealing. In addition to the above refractory filler, ⁇ -eucryptite, quartz glass, etc. may be added.
- a transition metal oxide such as CuO or Fe 2 O 3
- a refractory filler powder particularly cordierite
- the average particle size D 50 of the refractory filler is preferably less than 2 ⁇ m, in particular less than 1.5 ⁇ m.
- the average particle diameter D 50 of the refractory filler is less than 2 ⁇ m, the surface smoothness of the sealing material layer is improved and the average thickness of the sealing material layer is easily regulated to less than 10 ⁇ m. The accuracy of wearing can be increased.
- Maximum particle diameter D 99 of the refractory filler is preferably less than 5 [mu] m, 4 [mu] m or less, particularly 3 ⁇ m or less.
- the maximum particle diameter D 99 of the refractory filler is less than 5 [mu] m, together with the surface smoothness of the sealing material layer is improved, easily regulate the average thickness of the sealing material layer less than 10 [mu] m, as a result, the laser sealing The accuracy of wearing can be increased.
- “average particle diameter D 50 ” and “maximum particle diameter D 99 ” indicate values measured on a volume basis by a laser diffraction method.
- the thermal expansion coefficient of the sealing material is preferably 60 ⁇ 10 ⁇ 7 to 95 ⁇ 10 ⁇ 7 / ° C., 60 ⁇ 10 ⁇ 7 to 85 ⁇ 10 ⁇ 7 / ° C., in particular 65 ⁇ 10 ⁇ 7 to 80 ⁇ 10 ⁇ 7 / ° C.
- the thermal expansion coefficient is a value measured with a push rod type TMA apparatus in a temperature range of 30 to 300 ° C.
- the difference in thermal expansion coefficient between the ceramic substrate and the sealing material layer is preferably less than 45 ⁇ 10 ⁇ 7 / ° C., particularly preferably not more than 30 ⁇ 10 ⁇ 7 / ° C., and the thermal expansion coefficient between the sealing material layer and the glass substrate is 45 ⁇ 10 It is preferably less than ⁇ 7 / ° C., particularly 30 ⁇ 10 ⁇ 7 / ° C. or less. If the difference between the thermal expansion coefficients is too large, the stress remaining in the sealed portion is unduly high, and the long-term reliability of the hermetic package may be reduced.
- the softening point of the sealing material is preferably 500 ° C. or lower, 480 ° C. or lower, particularly 450 ° C. or lower.
- the lower limit of the softening point is not particularly set, but considering the thermal stability of the glass, the softening point is preferably 350 ° C. or higher.
- the “softening point” is the fourth inflection point when measured with a macro DTA apparatus, and corresponds to Ts in FIG.
- the sealing material may further contain a laser absorbing material in order to enhance the light absorption characteristics, but the laser absorbing material has an action of promoting devitrification of the bismuth-based glass. Therefore, the content of the laser absorbing material is preferably 0 to 15% by volume, 0 to 12% by volume, particularly 0 to 10% by volume. If the content of the laser absorbing material is more than 15% by volume, the glass tends to be devitrified at the time of laser sealing.
- Cu-based oxides, Fe-based oxides, Cr-based oxides, Mn-based oxides and spinel complex oxides thereof can be used as the laser absorber, and in particular, from the viewpoint of compatibility with bismuth-based glass. Therefore, a Mn-based oxide is preferable.
- the content is 0.1 volume% or more, 0.5 volume% or more, 1 volume% or more, 1.5 volume% or more, and especially 2 volume% or more is preferable.
- the sealing material layer may be formed after the member is mounted on the ceramic substrate, but from the viewpoint of preventing thermal deterioration of the member (particularly an element that is easily thermally deteriorated), before the member is mounted on the ceramic substrate. It is preferable to carry out.
- the average thickness of the sealing material layer after forming the sealing material layer on the ceramic substrate is less than 10 ⁇ m, less than 7 ⁇ m, particularly less than 5 ⁇ m.
- the average thickness of the sealing material layer after laser sealing is preferably regulated to less than 10 ⁇ m, less than 7 ⁇ m, and particularly less than 5 ⁇ m.
- the smaller the average thickness of the sealing material layer the lower the stress remaining in the sealing part after laser sealing, even if the thermal expansion coefficients of the sealing material layer and the ceramic substrate and the glass substrate are not sufficiently matched. .
- the accuracy of laser sealing can be increased.
- the method for regulating the average thickness of the sealing material layer includes a method of thinly applying the sealing material paste, and a method of polishing the surface of the sealing material layer after forming the sealing material layer. Can be mentioned.
- the surface roughness Ra of the sealing material layer after forming the sealing material layer on the ceramic substrate is less than 0.5 ⁇ m and 0.2 ⁇ m or less, particularly 0.01 to 0.15 ⁇ m. Further, it is preferable to regulate the surface roughness RMS of the sealing material layer after forming the sealing material layer on the ceramic substrate to less than 1.0 ⁇ m and 0.5 ⁇ m or less, particularly 0.05 to 0.3 ⁇ m. By doing so, the adhesion between the glass substrate and the sealing material layer is improved, and the accuracy of laser sealing is improved.
- methods for regulating the surface roughness Ra and RMS of the sealing material layer include a method for polishing the top of the frame portion of the ceramic substrate, a method for regulating the particle size of the refractory filler powder, and sealing. There is a method of polishing the surface of the material layer.
- the manufacturing method of the hermetic package of the present invention includes the steps of preparing a glass substrate and arranging the ceramic substrate and the glass substrate so that the glass substrate is in contact with the sealing material layer on the ceramic substrate.
- Various glasses can be used as the glass substrate.
- alkali-free glass, borosilicate glass, and soda lime glass can be used.
- alkali-free glass is suitable from the viewpoint of weather resistance.
- the plate thickness of the glass substrate is preferably 0.01 to 2.0 mm, 0.1 to 1 mm, and particularly preferably 0.5 to 0.7 mm. Thereby, thickness reduction of an airtight package can be achieved.
- the glass substrate may be disposed below the ceramic substrate, but it is preferable to dispose the glass substrate above the ceramic substrate from the viewpoint of laser sealing efficiency.
- the method for manufacturing an airtight package of the present invention is a process of irradiating a sealing material layer with laser light from the glass substrate side, and sealing the ceramic substrate and the glass substrate through the sealing material layer to obtain an airtight package.
- a semiconductor laser a YAG laser, a CO 2 laser, an excimer laser, an infrared laser, and the like are preferable in terms of easy handling.
- the atmosphere for laser sealing is not particularly limited, and may be an air atmosphere or an inert atmosphere such as a nitrogen atmosphere.
- FIG. 2 is a schematic cross-sectional view for explaining an embodiment of the hermetic package of the present invention.
- a member (piezoelectric vibrator element) 11 is formed in the central region of a rectangular ceramic base 10, and the outer peripheral edge region of the ceramic base 10 surrounds the periphery of the member 11 in a frame shape.
- a sealing material layer 12 is formed on the surface.
- the sealing material layer 12 is formed by applying and drying a sealing material paste, followed by sintering.
- the ceramic substrate 10 is formed with an electrode film (not shown) that electrically connects the member 11 and the outside.
- the glass substrate 13 is arrange
- the laser beam L emitted from the laser irradiation device 14 is irradiated along the sealing material layer 12 from the glass substrate 13 side.
- the sealing material layer 12 softens and flows, the ceramic base 10 and the glass substrate 13 are sealed, and the hermetic structure of the hermetic package 1 is formed.
- FIG. 3 is a schematic cross-sectional view for explaining an embodiment of the hermetic package of the present invention.
- the hermetic package 2 has a frame portion 21 in an outer peripheral edge region of a rectangular ceramic substrate 20, and a member (resin in which quantum dots are dispersed) 22 is accommodated therein.
- a sealing material layer 24 is formed on the top portion 23 of the frame portion 21.
- the ceramic substrate 20 is produced by sintering a laminate of green sheets.
- the top portion 23 of the frame portion 21 is previously polished, and the surface roughness Ra is 0.15 ⁇ m or less.
- the sealing material layer 24 is formed by applying and drying a sealing material paste and then sintering.
- the ceramic base 20 is formed with an electrode film (not shown) that electrically connects the member 22 and the outside.
- the glass substrate 25 is disposed above the ceramic substrate 20 so as to be in contact with the sealing material layer 24. Further, the laser beam L emitted from the laser irradiation device 26 is irradiated along the sealing material layer 24 from the glass substrate 25 side. As a result, the sealing material layer 24 softens and flows, the ceramic base 20 and the glass substrate 24 are sealed, and the hermetic structure of the hermetic package 2 is formed.
- a sealing material was prepared.
- Table 1 shows the material structure of the sealing material.
- Bismuth-based glass has a glass composition of mol%, Bi 2 O 3 76.5%, B 2 O 3 8.0%, ZnO 6.0%, CuO 5.0%, Fe 2 O 3 0.5. %, BaO 4.0%, and have the particle sizes listed in Table 1.
- the glass transition point is a value measured with a push rod type TMA apparatus.
- Softening point is a value measured with a macro DTA apparatus. The measurement was performed in an air atmosphere at a temperature rising rate of 10 ° C./min, and the measurement was performed from room temperature to 600 ° C.
- the thermal expansion coefficient is a value measured with a push rod type TMA apparatus.
- the measurement temperature range is 30 to 300 ° C.
- a sealing material layer was formed on the ceramic substrate using the sealing material (Sample Nos. 1 to 6).
- the sealing material vehicle, and solvent shown in Table 1 so that the viscosity is about 100 Pa ⁇ s (25 ° C., Shear rate: 4), until the powder is uniformly dispersed with a three-roll mill. Kneaded and pasted. A vehicle in which an ethyl cellulose resin was dissolved in a glycol ether solvent was used.
- the above-mentioned sealing material paste has a thickness of about 5 ⁇ m or about 8 ⁇ m, and a width of about 0.1 mm. It was printed in a frame shape with a screen printer so as to be 3 mm. Furthermore, after drying at 120 ° C. for 10 minutes in an air atmosphere, firing is performed at 500 ° C. for 10 minutes in an air atmosphere to incinerate (debinder treatment) and seal the resin component in the sealing material paste. The material was sintered (fixed) to form a sealing material layer on the ceramic substrate. Thereafter, an element was formed in the central region of the ceramic substrate. As a comparative example, a sealing material was formed on a glass substrate under the same firing conditions (Sample Nos. 7 to 9).
- the average thickness of the sealing material layer is a value measured with a non-contact type laser film thickness meter.
- the output and scanning speed described in the table are applied along the sealing material layer from the glass substrate side.
- the sealing material layer was softened and fluidized to seal the ceramic substrate and the glass substrate, and airtight packages described in Tables 2 and 3 were obtained.
- HAST test Highly Accelerated Temperature and Humidity Stress test
- the peelability was evaluated as “x” where peeling was recognized.
- the conditions of the HAST test are 121 ° C., humidity 100%, 2 atm, and 24 hours.
- the hermetic package of the present invention can be suitably applied to a piezoelectric vibrator package, but besides that, an airtight package that houses a light emitting diode, or a hermetic package that contains a resin in which quantum dots with low heat resistance are dispersed, etc.
- the present invention can also be suitably applied.
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Abstract
Description
10、20 セラミック基体
11、22 部材
12、24 封着材料層
13、25 ガラス基板
14、26レーザー照射装置
21 枠部
23 枠部の頂部
L レーザー光
Claims (10)
- セラミック基体を用意すると共に、セラミック基体上に封着材料層を形成する工程と、
ガラス基板を用意すると共に、ガラス基板がセラミック基体上の封着材料層に接触するように、セラミック基体とガラス基板を配置する工程と、
レーザー光をガラス基板側から封着材料層に向けて照射し、封着材料層を介してセラミック基体とガラス基板を封着して、気密パッケージを得る工程と、を備えることを特徴とする気密パッケージの製造方法。 - 基部と基部上に設けられた枠部とを有するセラミック基体を用い、枠部の頂部に封着材料層を形成することを特徴とする請求項1に記載の気密パッケージの製造方法。
- 枠部の頂部を研磨処理した後に、封着材料層を形成することを特徴とする請求項2に記載の気密パッケージの製造方法。
- 枠部の頂部の表面粗さRaが0.5μm未満になるように、枠部の頂部を研磨処理することを特徴とする請求項2又は3に記載の気密パッケージの製造方法。
- 封着材料ペーストを塗布、焼成して、セラミック基体上に封着材料の焼結体からなる封着材料層を形成することを特徴とする請求項1~4の何れかに記載の気密パッケージの製造方法。
- 55~95体積%のビスマス系ガラスと5~45体積%の耐火性フィラーを含有する封着材料を用いることを特徴とする請求項5に記載の気密パッケージの製造方法。
- 封着材料層の平均厚みを10μm未満とすることを特徴とする請求項1~6の何れかに記載の気密パッケージの製造方法。
- セラミック基体と封着材料層の熱膨張係数の差を45×10-7/℃未満とし、且つ封着材料層とガラス基板の熱膨張係数の差を45×10-7/℃未満とすることを特徴とする請求項1~7の何れかに記載の気密パッケージの製造方法。
- グリーンシートの積層体を焼結して、セラミック基体を作製することを特徴とする請求項1~8の何れかに記載の気密パッケージの製造方法。
- 請求項1~9の何れかに記載の気密パッケージの製造方法により作製されてなることを特徴とする気密パッケージ。
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