WO2018056210A1 - 複合基板,その製法及び電子デバイス - Google Patents
複合基板,その製法及び電子デバイス Download PDFInfo
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- WO2018056210A1 WO2018056210A1 PCT/JP2017/033454 JP2017033454W WO2018056210A1 WO 2018056210 A1 WO2018056210 A1 WO 2018056210A1 JP 2017033454 W JP2017033454 W JP 2017033454W WO 2018056210 A1 WO2018056210 A1 WO 2018056210A1
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- Prior art keywords
- substrate
- support substrate
- composite
- bonding
- sialon
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- 239000002131 composite material Substances 0.000 title claims abstract description 63
- 238000004519 manufacturing process Methods 0.000 title claims description 18
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- 239000010410 layer Substances 0.000 description 11
- WSMQKESQZFQMFW-UHFFFAOYSA-N 5-methyl-pyrazole-3-carboxylic acid Chemical compound CC1=CC(C(O)=O)=NN1 WSMQKESQZFQMFW-UHFFFAOYSA-N 0.000 description 10
- 239000000203 mixture Substances 0.000 description 8
- 238000010897 surface acoustic wave method Methods 0.000 description 8
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 238000005498 polishing Methods 0.000 description 6
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- 238000010304 firing Methods 0.000 description 5
- GQYHUHYESMUTHG-UHFFFAOYSA-N lithium niobate Chemical compound [Li+].[O-][Nb](=O)=O GQYHUHYESMUTHG-UHFFFAOYSA-N 0.000 description 5
- 239000000463 material Substances 0.000 description 5
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- 239000010980 sapphire Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
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- 239000000395 magnesium oxide Substances 0.000 description 4
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- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 4
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- 238000012360 testing method Methods 0.000 description 4
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910002601 GaN Inorganic materials 0.000 description 1
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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Definitions
- the present invention relates to a composite substrate, a manufacturing method thereof, and an electronic device.
- acoustic wave elements are used as band-pass filters in communication devices such as mobile phones.
- a piezoelectric substrate which is a surface acoustic wave element is required to have a high sound speed and a large electromechanical coupling coefficient. Therefore, lithium niobate (LN) and lithium tantalate (LT) satisfying the requirements are widely used. Yes.
- LN lithium niobate
- LT lithium tantalate
- LT and LN have a large coefficient of thermal expansion and a large amount of expansion and contraction due to environmental temperature changes. As a result, the center frequency of the filter is shifted, so that the passing frequency is reduced and the characteristics are deteriorated. For this reason, it has become necessary that the surface acoustic wave device hardly expands and contracts due to environmental temperature changes.
- Patent Document 1 discloses a composite substrate in which a piezoelectric substrate and a support substrate are bonded via an adhesive layer. Further, sapphire, silicon, alumina and the like are exemplified as the material of the support substrate. Since these materials have a smaller thermal expansion coefficient than that of the piezoelectric substrate, the frequency temperature dependency can be lowered, and since the sound speed is high, they are suitable for high-frequency surface acoustic wave elements.
- Patent Document 2 a 0.1 to 10 ⁇ m amorphous layer is formed on a supporting substrate by a CVD method or the like, and then the supporting substrate and the single crystal semiconductor substrate are connected via the amorphous layer. A method of obtaining a composite substrate by bonding is illustrated. Examples of the material of the support substrate include sialon.
- sapphire and alumina of Patent Document 1 have a problem that the frequency temperature dependency cannot be significantly reduced because the coefficient of thermal expansion is about 7 ppm / K even though the coefficient of thermal expansion is smaller than that of the piezoelectric substrate. .
- sapphire has a problem of poor workability because its Young's modulus is too high at 450 GPa or more.
- silicon has a sufficiently small coefficient of thermal expansion compared to a piezoelectric substrate, but its Young's modulus is as low as about 180 to 190 GPa, so warping and cracking occur, and even a high resistivity is in the order of 10 4 ⁇ cm. There is a problem that the resonance characteristics of the filter deteriorate due to lack of insulation.
- Patent Document 2 exemplifies sialon as a material for the support substrate.
- the composite substrate of Patent Document 2 has an amorphous layer having a low Young's modulus of 0.1 to 10 ⁇ m between the support substrate and the single crystal semiconductor substrate, the Young's modulus of the entire composite substrate is still too low.
- the restraining force of the piezoelectric substrate by the support substrate cannot be sufficiently expressed.
- the present invention has been made to solve such a problem, and has as its main object to provide a composite substrate suitable as a material for a high-frequency acoustic wave device.
- the composite substrate of the present invention is a composite substrate in which a support substrate and a functional substrate are directly bonded, and the support substrate is a sialon sintered body. Since the sialon sintered body has a high sound speed, the acoustic wave device using the composite substrate of the present invention can be used at a higher frequency. In addition, since the Young's modulus is an appropriate value for the sialon sintered body, the composite substrate of the present invention is less likely to warp or crack, but the workability is good. Furthermore, the sialon sintered body has a high resistivity. Since the insulating property is high, the acoustic wave device using the composite substrate of the present invention has good resonance characteristics.
- the acoustic wave device using the composite substrate of the present invention can sufficiently reduce the frequency temperature dependency.
- the support substrate and the functional substrate are integrated by direct bonding, the Young's modulus of the entire composite substrate may not be too low compared to the case where both substrates are integrated by an adhesive layer or the like. The restraining force of the functional substrate by the support substrate can be sufficiently expressed.
- the method for producing a composite substrate of the present invention is a method for manufacturing the composite substrate described above, and includes a bonding step of directly bonding the surface of the support substrate and the surface of the functional substrate, and before the bonding step, (A) Polishing the surface so that the number of pores existing on the surface of the support substrate is 30 or less per 100 ⁇ m ⁇ 100 ⁇ m area, or (b) 100 ⁇ m ⁇ 140 ⁇ m of the surface of the support substrate The surface is polished so that the center line average roughness (Ra) in the measurement range is 1 nm or less, or (c) the maximum peak height of the cross-sectional curve in the measurement range of 100 ⁇ m ⁇ 140 ⁇ m of the surface of the support substrate The surface is polished so that the height difference (Pt) from the maximum valley depth is 30 nm or less.
- the sialon sintered body since the sialon sintered body is used as the support substrate, the surface obtained by polishing the support substrate has high surface flatness. Therefore, it is suitable for directly bonding
- the electronic device of the present invention uses the above-described composite substrate of the present invention.
- the sialon sintered body that is the support substrate of this electronic device has a high sound speed, an appropriate Young's modulus, a high resistivity, and a sufficiently low thermal expansion coefficient. For this reason, this electronic device can be used at a higher frequency and is less likely to warp or crack, but has good workability, good resonance characteristics, and sufficiently low frequency temperature dependency.
- FIG. 1 is a perspective view of a composite substrate 10.
- the composite substrate of the present embodiment is a composite substrate in which a support substrate and a functional substrate are directly bonded, and the support substrate is a sialon sintered body.
- the sialon sintered body is represented by the general formula: Si 6-z Al z O z N 8-z (0 ⁇ z ⁇ 4.2), but it dissolves a metal oxide such as magnesium oxide or yttrium oxide. It may be.
- the functional substrate is not particularly limited, and examples thereof include LT, LN, gallium nitride, and silicon. Of these, LT and LN are preferred.
- An amorphous layer having a thickness of 5 nm or less may exist at the interface between the support substrate and the functional substrate.
- the elastic wave device using the composite substrate of this embodiment can be used at a higher frequency.
- the sound speed of the sialon sintered body is preferably 5000 m / s or more, and more preferably 5500 m / s or more.
- the speed of sound is determined by the rigidity, density, Young's modulus, and Poisson's ratio, but Sialon can control these characteristics by adjusting the value of z in the above equation.
- the Sialon sintered body has an appropriate Young's modulus. That is, since the composite substrate of the present embodiment is reasonably hard, warpage and cracking hardly occur and workability is also good.
- the Young's modulus of the sialon sintered body is preferably 200 GPa or more and 350 GPa or less.
- Sialon sintered bodies have high resistivity and high insulation. For this reason, the acoustic wave device using the composite substrate of the present embodiment has good resonance characteristics.
- the resistivity of the sialon sintered body is preferably 10 14 ⁇ cm or more.
- the thermal expansion coefficient (40 to 400 ° C.) of the sialon sintered body is preferably 3.0 ppm / K or less, and more preferably 2.7 ppm / K or less.
- the sialon sintered body preferably has an open porosity of 0.1% or less and a relative density of 99.9% or more.
- the sintered sialon preferably has a ratio of the sum of the maximum peak intensities of components other than sialon to the maximum peak intensity of sialon in the X-ray diffraction diagram of 0.005 or less.
- the manufacturing flow of the sialon sintered body includes a step of producing a sialon raw material powder and a step of producing a sialon sintered body.
- each powder is more preferably fine, and an average particle size is preferably 1.5 ⁇ m or less, more preferably 1 ⁇ m or less.
- the mixing method of the raw material powder is not particularly limited, and for example, a ball mill, an attritor, a bead mill, a jet mill or the like can be used, and either a dry method or a wet method may be used. However, a wet method using a solvent is preferable to obtain a homogeneously mixed raw material powder. In that case, the solvent used for mixing is removed by drying to obtain a raw material powder.
- the raw material powder may contain an additive. Examples of the additive include magnesium oxide and yttrium oxide.
- the obtained slurry is dried, and the dried product is passed through a sieve to obtain sialon raw material powder.
- a composition suitably etc. to make raw material powder when a composition shifts by mixing of a media component etc. at the time of mixing.
- the mixture may be used as the sialon raw material powder as it is by adjusting the mass of each component of the mixed powder in advance so that the mass of each component contained in the mixture has a desired sialon composition.
- the obtained sialon raw material powder is formed into a predetermined shape.
- molding method can be used.
- the sialon raw material powder as described above may be press-molded with a mold as it is. In the case of press molding, if the sialon raw material powder is granulated by spray drying, the moldability is improved.
- an organic binder can be added to produce clay and extrusion molding, or a slurry can be produced and sheet molded. In these processes, it is necessary to remove the organic binder component before or during the firing step. Further, high pressure molding may be performed by CIP (cold isostatic pressing).
- the obtained compact is fired to produce a sialon sintered body.
- a hot press method is very effective as the method. By using the hot press method, densification progresses in a fine grain state at a low temperature compared to normal pressure sintering, and the residual coarse pores often seen in normal pressure sintering can be suppressed.
- the firing temperature during hot pressing is preferably 1725 to 1900 ° C, more preferably 1750 to 1900 ° C. Further, it is preferable that the press pressure during hot pressing and 100 ⁇ 300kgf / cm 2, more preferably 150 ⁇ 250kgf / cm 2.
- the holding time at the firing temperature can be appropriately selected in consideration of the shape and size of the molded body and the characteristics of the heating furnace.
- a specific preferable holding time is, for example, 1 to 12 hours, and more preferably 2 to 8 hours.
- the firing atmosphere during hot pressing is preferably a nitrogen atmosphere in order to avoid decomposition of sialon.
- This manufacturing method preferably includes a step of directly bonding the surface of the support substrate made of the sialon sintered body and the surface of the functional substrate.
- the ratio of the actual bonded area (bonded area ratio) in the bonding interface is preferably 80% or more, and more preferably 90% or more. When the bonding area ratio is large as described above, a good composite substrate in which the functional substrate and the support substrate are firmly bonded is obtained.
- the two substrates are pressed with the bonding surfaces facing each other.
- the bonding surface is activated by, for example, irradiation of a neutral atom beam of an inert gas (such as argon) to the bonding surface, or irradiation of plasma or ion beam.
- a neutral atom beam of an inert gas such as argon
- irradiations can be performed using, for example, an ion gun or a FAB gun.
- a FAB gun has a higher energy per particle than an ion gun, and has a high ability to remove an oxide film and an adsorption layer on the substrate surface that interfere with room temperature bonding.
- the FAB gun is more preferable because it is easy to make a free joint necessary for joining.
- the surface is polished and finished so that the number of pores existing on the surface of the support substrate is 30 or less per 100 ⁇ m ⁇ 100 ⁇ m area, or (b 1) Polish the surface so that the center line average roughness (Ra) in the measurement range of 100 ⁇ m ⁇ 140 ⁇ m of the support substrate surface is 1 nm or less, or (c) In the measurement range of 100 ⁇ m ⁇ 140 ⁇ m of the support substrate surface.
- the surface is preferably polished so that the difference in height (Pt) between the maximum peak height and the maximum valley depth of the cross-sectional curve is 30 nm or less.
- the bonding area ratio can be 80% or more (preferably 90% or more).
- the number of pores in (a) described above is more preferably 10 or less, Ra in (b) described above is more preferably 0.9 nm or less, and Pt in (c) described above is more preferably 27 nm or less.
- the polishing finish on the surface of the support substrate is preferably performed so as to satisfy at least one of (a) to (c). Further, the surface of the functional substrate is preferably polished so as to satisfy at least one of (a) to (c) similarly to the surface of the support substrate.
- FIG. 1 shows an example of a composite substrate.
- the composite substrate 10 is obtained by bonding a piezoelectric substrate 12 which is a functional substrate and a support substrate 14 by direct bonding.
- the composite substrate produced in this way is directly bonded, the Young's modulus of the entire composite substrate does not become too low compared to the case of bonding via an adhesive layer, and the functionality of the support substrate Since the binding force of the substrate is strong, the frequency temperature dependency can be reduced.
- the composite substrate manufactured in this manner may have an amorphous layer having a thickness of 5 nm or less at the interface between the support substrate and the functional substrate. Even if such an extremely thin amorphous layer exists between the support substrate and the functional substrate, the Young's modulus of the entire composite substrate does not become too low, and the binding force of the functional substrate by the support substrate is not reduced. It can be fully expressed.
- the electronic device uses the composite substrate described above.
- the composite substrate used for the electronic device preferably has a ratio of the thickness of the functional substrate to the support substrate (the thickness of the functional substrate / the thickness of the support substrate) of 0.1 or less.
- Examples of such electronic devices include acoustic wave devices (surface acoustic wave devices, Lamb wave elements, thin film resonators (FBAR), etc.), LED devices, optical waveguide devices, switch devices, and the like.
- FIG. 2 shows an example of an electronic device 30 manufactured using the composite substrate 10.
- the electronic device 30 is a 1-port SAW resonator, that is, a surface acoustic wave device.
- a pattern of a large number of electronic devices 30 is formed on the piezoelectric substrate 12 of the composite substrate 10 using a general photolithography technique, and then cut into individual electronic devices 30 by dicing.
- the electronic device 30 is a device in which comb-shaped IDT (Interdigital Transducer) electrodes 32 and 34 and a reflective electrode 36 are formed on the surface of the piezoelectric substrate 12 by a photolithography technique.
- IDT Interdigital Transducer
- the raw material powder includes commercially available silicon nitride powder (oxygen content 1.3 mass%, impurity metal element content 0.2 mass% or less, average particle size 0.6 ⁇ m), aluminum nitride (oxygen content) 0.8 mass%, impurity metal element content 0.1 mass% or less, average particle diameter 1.1 ⁇ m), alumina (purity 99.9 mass%, average particle diameter 0.5 ⁇ m), silica (purity 99.9 mass) %, Average particle size 0.5 ⁇ m).
- the sialon raw material powders A to K were produced as follows. That is, first, each powder of aluminum nitride, alumina, silicon nitride, and silica was weighed so as to have a sialon composition (Si 6 -z Al z O z N 8 -z ) having the value of z shown in Table 1. These powders were mixed with alumina cobblestone ( ⁇ 5 mm) in a ball mill using isopropyl alcohol as a solvent for 4 hours to prepare a sialon mixture (slurry mixed with powder). The obtained slurry was dried at 110 ° C. under a nitrogen gas flow, and the dried product was passed through a sieve to obtain sialon raw material powders A to K.
- magnesium oxide (purity 99.9%, average particle size 1.8 ⁇ m) is used for sialon raw material powders D, H, and K, and yttrium oxide (purity 99.9 is used for sialon raw material powders E, F, G, I, and J). % And average particle diameter of 1.1 ⁇ m).
- the properties of the sintered body surface were evaluated by polishing one surface of a test piece of about 4 mm ⁇ 3 mm ⁇ 10 mm into a mirror surface by polishing.
- the polishing was performed by lapping 3 ⁇ m diamond abrasive grains and finally 0.5 ⁇ m diamond abrasive grains.
- Relative density was calculated as bulk density / apparent density.
- the sialon sintered body was pulverized, and sialon and heterophase were identified and the maximum peak intensity of each phase was calculated using an X-ray diffractometer. Since the alumina mortar is used for pulverization of the sintered body, there is a possibility that alumina will be mixed from the alumina mortar, and caution is required for pulverization for a long time.
- sialon sintered grains on the fracture surface were observed with a SEM in a 127 ⁇ m ⁇ 88 ⁇ m field of view, and the particle diameters of 10 or more sialon sintered grains in the field of view were obtained. It was set as the average particle diameter of the sialon sintered grain. In addition, the particle size of one sialon sintered grain was the average value of the major axis and minor axis of the sintered grain.
- Number of pores Observe the mirror-finished surface as described above with a 3D measurement laser microscope, and count the count value per unit area of pores with a maximum length of 0.5 ⁇ m or more and a depth of 0.08 ⁇ m or more. The average value was taken as the number of pores.
- the unit area was an area of 100 ⁇ m square.
- Ra and Pt in the present specification correspond to the arithmetic mean roughness Ra of the cross-sectional curve and the maximum cross-sectional height Pt of the cross-sectional curve defined by JIS B 0601: 2013.
- the above Ra and Pt were defined as surface flatness.
- the measurement range was 100 ⁇ m ⁇ 140 ⁇ m.
- test piece was a 3 mm ⁇ 4 mm ⁇ 40 mm bending rod.
- CTE 40-400 ° C
- the sound velocity c was calculated by the following formula.
- the Poisson's ratio was measured by attaching a strain gauge to the test piece.
- c (G / ⁇ ) 1/2
- G E / 2 (1 + ⁇ )
- G rigidity
- ⁇ density
- E Young's modulus
- ⁇ Poisson's ratio
- the sialon sintered body of Experimental Example 1 had excellent characteristics. Specifically, the bulk density of the sialon sintered body of Experimental Example 1 was 3.160 g / cm 3 , the open pores were 0.00%, and the relative density was 100.00%. In addition to sialon, slight alumina and silicon oxynitride were detected in the crystal phase. The ratio (peak intensity ratio) Ix of the sum of the maximum peak intensities of the respective components other than sialon to the maximum peak intensity of sialon was 0.0012, which was extremely small. In the 100 ⁇ m ⁇ 100 ⁇ m range of the polished surface, the number of pores having a maximum length of 0.5 ⁇ m or more was one and very small.
- the centerline average roughness Ra was as small as 0.4 nm, and the difference Pt between the maximum peak height and the maximum valley depth of the cross-sectional curve was as small as 15 nm.
- the Young's modulus was 307 GPa, the thermal expansion coefficient (40 to 400 ° C.) was 2.7 ppm / K, and the sound velocity was 6200 m / s.
- the resistivity of the sialon sintered body of Experimental Example 1 exceeded 10 14 ⁇ cm, and the insulation was high.
- the number of pores is 10 or less, the center line average roughness Ra is 1.0 nm or less, the height difference Pt between the maximum peak height and the maximum valley depth is 30 nm or less, the Young's modulus is 210 GPa or more, and the CTE is 3.0 ppm / K.
- the sound speed was 5000 m / s or more, and excellent characteristics were provided.
- the resistivity of the sialon sintered bodies of Experimental Examples 2 to 11 exceeded 10 14 ⁇ cm.
- the sialon sintered bodies of Experimental Examples 4 to 11 are those in which magnesium oxide or yttrium oxide is dissolved in sialon, and all of them have the same characteristics as the sialon sintered bodies of Experimental Examples 1 to 3. I understood it.
- an LT substrate having a diameter of about 100 mm and a thickness of about 250 ⁇ m is directly applied to a support substrate having a diameter of about 100 mm and a thickness of about 230 ⁇ m cut out from the sintered bodies of Experimental Examples 1 to 11, respectively.
- the composite substrate was obtained by bonding.
- the activation process of the surface before joining was performed. Specifically, after evacuating to the 10 ⁇ 6 Pa level, both substrates were irradiated with a neutral atom beam of argon (acceleration voltage: 1 kV, current: 100 mA, Ar flow rate: 50 sccm) using a FAB gun for 120 sec. Thereafter, the two substrates were bonded together and pressed with a bonding load of 0.1 ton for 1 minute, and the support substrate and the LT substrate were directly bonded at room temperature.
- the composite substrates of Experimental Examples 12 to 22 use a support substrate with small Ra and Pt, and almost no bubbles are observed at the bonding interface between the support substrate and the LT substrate, and the actual bonding area of the bonding interface.
- the ratio (bonded area ratio) was 92% or more as shown in Table 3, and was well bonded.
- the bonding area is the area of the portion without bubbles
- the bonding area ratio is the ratio of the bonding area to the area of the entire bonding interface.
- the composite substrate bonded well in Experimental Examples 12 to 22 does not peel off even when the LT substrate side is polished to a thickness of several ⁇ m to 20 ⁇ m, and the bonded area is maintained at 92% or more.
- the support substrate and the LT substrate were bonded very firmly. Further, the cross section of the bonding interface was observed with a transmission electron microscope (TEM). There was no gap at the bonding interface, and there was a very thin amorphous layer that was firmly bonded even at the atomic level.
- the thickness of the amorphous layer was measured using Experimental Examples 7 to 9 as representative examples, which were 3.6 nm, 3.8 nm, and 4.1 nm, respectively. The thickness of the amorphous layer was an average value measured at three different locations of the amorphous layer.
- the conventional silicon support substrate (Young's modulus: 190 GPa, thermal expansion coefficient: about 4 ppm / K, resistivity 10 4 ⁇ cm level) has a lower Young's modulus than the sialon support substrate, so the binding force of the functional substrate is low.
- the functional substrate is easily expanded and contracted because it is small and has a large thermal expansion coefficient, and the resonance characteristics are likely to deteriorate because the resistivity is low.
- the conventional alumina support substrate (Young's modulus: 370 GPa, thermal expansion coefficient: about 7 ppm / K) and sapphire support substrate (Young's modulus: 490 GPa, thermal expansion coefficient: about 7 ppm / K) have a thermal expansion coefficient of sialon.
- the functional substrate tends to expand and contract.
- TCF frequency-temperature characteristics
- experimental examples 12 to 22 described above correspond to examples of the composite substrate and the manufacturing method thereof according to the present invention.
- the present invention is applicable to electronic devices such as Lamb wave elements and thin film resonators (FBARs) in addition to surface acoustic wave elements.
- FBARs thin film resonators
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Abstract
Description
原料粉末には、不純物金属元素含有量が0.2質量%以下、平均粒径が2μm以下の市販の窒化珪素、窒化アルミニウム、アルミナ及びシリカ粉末を用いた。これら原料を用いて、Si:Al:O:N=(6-z):z:z:(8-z)(但し0<z≦4.2)が所定組成となるように質量割合を決定して各成分を混合してサイアロン原料粉末を作製する。zの値は0.5≦z≦4.0が好ましい。各粉末は、緻密に焼結するためには細かいものがより好ましく、平均粒径が1.5μm以下、更には1μm以下のものが好ましい。原料粉末の混合方法に特に制限はなく、例えばボールミル、アトライター、ビーズミル、ジェットミル等を利用することができ、乾式、湿式どちらの混合方法でもよい。但し、均質に混合された原料粉末を得るには溶媒を用いた湿式法が好ましい。その場合、混合に用いた溶媒等は乾燥除去されることで原料粉末を得る。原料粉末には添加物が含まれていてもよい。添加物としては、酸化マグネシウムや酸化イットリウムなどが挙げられる。得られたスラリーを乾燥し、乾燥物を篩に通してサイアロン原料粉末とする。なお、混合時にメディア成分等の混入によって組成がずれた場合は、適宜組成調整するなどして原料粉末とすればよい。あるいは、混合物に含まれる各成分の質量が所望のサイアロン組成になるように、予め混合粉末の各成分の質量を調整しておくことにより、混合物をそのままサイアロン原料粉末としてもよい。
得られたサイアロン原料粉末を所定形状に成形する。成形の方法に特に制限はなく、一般的な成形法を用いることができる。例えば、上記のようなサイアロン原料粉末をそのまま金型によってプレス成形してもよい。プレス成形の場合は、サイアロン原料粉末をスプレードライによって顆粒状にしておくと、成形性が良好になる。他に、有機バインダーを加えて坏土を作製し押出し成形したり、スラリーを作製しシート成形することができる。これらのプロセスでは焼成工程前あるいは焼成工程中に有機バインダー成分を除去することが必要になる。また、CIP(冷間静水圧プレス)にて高圧成形をしてもよい。
原料粉末には、市販の窒化珪素粉末(酸素含有量1.3質量%、不純物金属元素含有量0.2質量%以下、平均粒径0.6μm)、窒化アルミニウム(酸素含有量0.8質量%、不純物金属元素含有量0.1質量%以下、平均粒径1.1μm)、アルミナ(純度99.9質量%、平均粒径0.5μm)、シリカ(純度99.9質量%、平均粒径0.5μm)の粉末を用いた。
(1)実験例1
実験例1のサイアロン焼結体は、サイアロン原料粉末Aを金型を用いて直径125mm、厚さ約20mmに成形した後、黒鉛型にて、プレス圧力200kgf/cm2下、最高温度1800℃で4時間、ホットプレス焼成したものである。焼成雰囲気は、窒素雰囲気とした。得られた焼結体は直径125mmで厚さは約8mmであった。この焼結体から4mm×3mm×40mmサイズの抗折棒などを切り出し、各種特性を評価した。各種特性の評価方法を以下に示す。また、結果を表2に示す。なお、焼結体表面の性状は、4mm×3mm×10mm程度の試験片の一面を研磨によって鏡面状に仕上げて評価した。研磨は3μmのダイヤモンド砥粒、最終的に0.5μmのダイヤモンド砥粒のラップ研磨を行った。
蒸留水を用いたアルキメデス法により測定した。
相対密度は嵩密度÷見掛け密度で算出した。
サイアロン焼結体を粉砕し、X線回折装置により、サイアロン、異相の同定と各相の最大ピークの強度の算出を行った。焼結体の粉砕は、アルミナ乳鉢を用いているためアルミナ乳鉢からアルミナが混合される可能性があり、長時間の粉砕には注意が必要である。XRD装置には、全自動多目的X線解析装置D8 ADVANCEを用い、CuKα、40kV、40mA、2θ=10-70°を測定条件とした。X線回折図から、サイアロンの最大ピーク(2θ=32.8~33.5°)の強度(Ic)に対する、検出された各異相(P、Q、R、・・・)の最大ピークの強度(Ip、Iq、Ir、・・・)の総和の比(ピーク強度比Ix)を下記式から求めた。なお、最大ピークが他のピークと重なる場合は、最大ピークの代わりに2番目にピーク強度の大きなピークを採用した。
Ix=(Ip+Iq+Ir・・・)/Ic
破断面におけるサイアロン焼結粒をSEMにて127μm×88μmの視野で観察し、視野内の10個以上のサイアロン焼結粒の粒径を求め、その平均値をサイアロン焼結粒の平均粒径とした。なお、1つのサイアロン焼結粒の粒径は、その焼結粒の長径と短径の平均値とした。
上記のように鏡面状に仕上げた面を3D測定レーザー顕微鏡で観察し、最大長さが0.5μm以上、深さが0.08μm以上の気孔の単位面積当たりの計数値を4箇所で計測し、その平均値を気孔数とした。単位面積は100μm四方の面積とした。
上記のように鏡面状に仕上げた面に対し、3次元光学プロファイラー(Zygo)を用いて中心線平均粗さRaと、最大山高さと最大谷深さとの高さの差Ptを測定した。本明細書中のRaとPtは、JIS B 0601:2013で規定される、断面曲線の算術平均粗さRaと断面曲線の最大断面高さPtに対応する。上記のRa、Ptを表面平坦性とした。測定範囲は、100μm×140μmとした。
JIS R1602に準じた、静的撓み法で測定した。試験片形状は3mm×4mm×40mm抗折棒とした。
JIS R1618に準じて、押し棒示差式で測定した。試験片形状は3mm×4mm×20mmとした。
音速cは、下記式により算出した。なお、ポアソン比は試験片にひずみゲージを貼付して測定した。
c=(G/ρ)1/2 ,G=E/2(1+ν)
(G:剛性率、ρ:密度、E:ヤング率、ν:ポアソン比)
実験例2~11のサイアロン焼結体は、サイアロン原料粉末Aの代わりに表1に示すサイアロン原料粉末B~Kを用いて、実験例1と同様にしてホットプレス焼成したものである。各サイアロン焼結体の特性を表2に示す。いずれのサイアロン焼結体も、開気孔率は0.01%以下、相対密度は99.9%以上、サイアロン以外の相とのピーク強度比Ixは0.005以下、サイアロン平均粒径は20μm以下、気孔数は10個以下、中心線平均粗さRaは1.0nm以下、最大山高さと最大谷深さとの高さの差Ptは30nm以下、ヤング率は210GPa以上、CTEは3.0ppm/K以下、音速は5000m/s以上であり、優れた特性を備えていた。また、実験例2~11のサイアロン焼結体の抵抗率はいずれも1014Ωcmを超えていた。なお、実験例4~11のサイアロン焼結体は、酸化マグネシウムあるいは酸化イットリウムがサイアロン中に固溶したものであるが、いずれも実験例1~3のサイアロン焼結体と同等の特性が得られることがわかった。
実験例12~22では、実験例1~11の焼結体からそれぞれ切り出した直径100mm、厚さ230μm程度の支持基板に、直径100mm、厚さ250μm程度のLT基板を直接接合して複合基板を得た。まず、接合前の表面の活性化処理を行った。具体的には、10-6Pa台まで真空引きした後、FABガンを用いてアルゴンの中性原子ビーム(加速電圧:1kV、電流:100mA、Ar流量:50sccm)を120sec両基板に照射した。その後、両基板を貼り合わせ、接合荷重0.1tonで1分間プレスし、支持基板とLT基板を室温で直接接合した。
Claims (10)
- 支持基板と機能性基板とが直接接合された複合基板であって、
前記支持基板は、サイアロン焼結体である、
複合基板。 - 前記支持基板と前記機能性基板との界面にアモルファス層があり、前記アモルファス層の厚さが5nm以下である、
請求項1に記載の複合基板。 - 支持基板と機能性基板とがアモルファス層を介して接合された複合基板であって、
前記アモルファス層の厚さが5nm以下である、
複合基板。 - 前記機能性基板は、圧電基板である、
請求項1~3のいずれか1項に記載の複合基板。 - 前記支持基板の音速が5000m/s以上である、
請求項1~4のいずれか1項に記載の複合基板。 - 前記支持基板の40~400℃の熱膨張係数が3.0ppm/K以下である、
請求項1~5のいずれか1項に記載の複合基板。 - 請求項1~6のいずれか1項に記載の複合基板を製造する方法であって、
前記支持基板の前記表面と前記機能性基板の表面とを直接接合によって接合する接合工程
を含み、
前記接合工程の前に、前記支持基板の表面に存在する気孔の数が100μm×100μmの面積当たり30個以下となるように前記表面を研磨仕上げする、
複合基板の製法。 - 請求項1~6のいずれか1項に記載の複合基板を製造する方法であって、
前記支持基板の表面と前記機能性基板の表面とを直接接合によって接合する接合工程
を含み、
前記接合工程の前に、前記支持基板の前記表面の100μm×140μmの測定範囲における中心線平均粗さ(Ra)が1nm以下となるように前記表面を研磨仕上げする、
複合基板の製法。 - 請求項1~6のいずれか1項に記載の複合基板を製造する方法であって、
前記支持基板の表面と前記機能性基板の表面とを直接接合によって接合する接合工程
を含み、
前記接合工程の前に、前記支持基板の前記表面の100μm×140μmの測定範囲における断面曲線の最大山高さと最大谷深さとの高さの差(Pt)が30nm以下となるように前記表面を研磨仕上げする、
複合基板の製法。 - 請求項1~6のいずれか1項に記載の複合基板を利用した電子デバイス。
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