WO2016060080A1 - ワークの貼り合わせ方法 - Google Patents
ワークの貼り合わせ方法 Download PDFInfo
- Publication number
- WO2016060080A1 WO2016060080A1 PCT/JP2015/078767 JP2015078767W WO2016060080A1 WO 2016060080 A1 WO2016060080 A1 WO 2016060080A1 JP 2015078767 W JP2015078767 W JP 2015078767W WO 2016060080 A1 WO2016060080 A1 WO 2016060080A1
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- WIPO (PCT)
- Prior art keywords
- workpiece
- workpieces
- bonding
- surface activation
- gas
- Prior art date
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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
- B32B2310/00—Treatment by energy or chemical effects
- B32B2310/04—Treatment by energy or chemical effects using liquids, gas or steam
- B32B2310/0445—Treatment by energy or chemical effects using liquids, gas or steam using gas or flames
- B32B2310/0463—Treatment by energy or chemical effects using liquids, gas or steam using gas or flames other than air
- B32B2310/0472—Treatment by energy or chemical effects using liquids, gas or steam using gas or flames other than air inert gas
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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
- B32B2310/00—Treatment by energy or chemical effects
- B32B2310/08—Treatment by energy or chemical effects by wave energy or particle radiation
- B32B2310/0806—Treatment by energy or chemical effects by wave energy or particle radiation using electromagnetic radiation
- B32B2310/0831—Treatment by energy or chemical effects by wave energy or particle radiation using electromagnetic radiation using UV radiation
-
- 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
- B32B2310/00—Treatment by energy or chemical effects
- B32B2310/14—Corona, ionisation, electrical discharge, plasma treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C2201/00—Manufacture or treatment of microstructural devices or systems
- B81C2201/01—Manufacture or treatment of microstructural devices or systems in or on a substrate
- B81C2201/0174—Manufacture or treatment of microstructural devices or systems in or on a substrate for making multi-layered devices, film deposition or growing
- B81C2201/019—Bonding or gluing multiple substrate layers
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N2035/00346—Heating or cooling arrangements
- G01N2035/00455—Controlling humidity in analyser
Definitions
- the present invention relates to a method for bonding workpieces made of synthetic resin, glass, silicon wafer, crystal or sapphire.
- This microreactor is composed of a microchip in which a microscale analysis channel or the like is formed on a small substrate made of, for example, silicon, silicone resin or glass by a semiconductor microfabrication technique.
- a reaction analysis system using such a microreactor is called a micro total analysis system (hereinafter referred to as “ ⁇ TAS”).
- ⁇ TAS micro total analysis system
- a chip suitable for various applications can be configured.
- Applications of the microchip include chemical analysis such as gene analysis, clinical diagnosis, drug screening, analysis in the fields of chemistry, pharmacy, medicine, medicine, veterinary medicine, compound synthesis, environmental measurement, and the like.
- Such a microchip typically has a structure in which a pair of substrates are bonded to face each other. Fine channels (for example, about 10 to several hundred ⁇ m in width and about 10 to several hundred ⁇ m in depth) are formed on the surface of at least one substrate.
- a glass substrate is mainly used because it is easy to manufacture and can be optically detected. Recently, development of a microchip using a resin substrate that is lightweight but is less likely to be damaged than a glass substrate and that is inexpensive.
- a method using an adhesive or a method using thermal fusion can be considered as a method for bonding substrates.
- these methods have the following problems.
- the adhesive oozes out into the micro flow path and the flow path is blocked, a part of the micro flow path becomes narrow and the flow path has a non-uniform diameter, There is a problem that the homogeneous characteristics of the road wall are disturbed.
- the method of bonding by heat fusion if the fusion is performed at a temperature higher than the heat melting temperature, the flow path may be collapsed in the heating stage, or the flow path may not be maintained in a predetermined cross-sectional shape. There is a problem that functionalization becomes difficult.
- the conventional bonding method has the following problems. That is, the illuminance of ultraviolet rays irradiated on the surfaces of the substrates, the substrate surface activation processing conditions such as the power for converting the process gas into plasma and the flow rate of the process gas, and the pressure applied when bonding the substrates together Even if the bonding processing conditions such as the heating temperature and the heating time are managed with high accuracy, the bonding state of the obtained bonded body varies, and it is difficult to reliably achieve a high strength bonding state.
- an object of the present invention is to provide a method for bonding workpieces that can achieve a high-strength bonding state and that can achieve good reproducibility of the bonding state.
- the workpiece bonding method of the present invention is a method of bonding two workpieces made of a material selected from the group consisting of synthetic resin, glass, silicon wafer, crystal and sapphire, A surface activation step for activating the bonding surface of at least one workpiece; A joining step of joining the two workpieces in a stacked state so that their bonding surfaces are in contact with each other; Before performing the surface activation step, a pretreatment step is performed in which moisture is released from the bonded surface of the workpiece used in the surface activation step.
- the pretreatment step is preferably performed by heating the workpiece to be subjected to the surface activation step.
- the said pretreatment process is performed by arrange
- the said pretreatment process is performed by spraying dry air or inert gas with respect to the bonding surface of the workpiece
- the said surface activation process is an ultraviolet irradiation process process which irradiates a vacuum ultraviolet-ray to the bonding surface of the said workpiece
- the said surface activation process is a plasma gas processing process which makes the process gas plasmified by atmospheric pressure plasma contact the bonding surface of the said workpiece
- the pretreatment step of the surface activation step moisture is released from the workpiece bonding surface, so that a high strength bonded state can be achieved, and the bonded state Good reproducibility can be obtained.
- the workpiece bonding method of the present invention is a method of bonding two plate-shaped workpieces, for example.
- the workpiece applied to the bonding method of the present invention is made of a material selected from the group consisting of synthetic resin, glass, silicon wafer, crystal and sapphire.
- a synthetic resin constituting the workpiece a silicone resin such as polydimethylsiloxane, a cycloolefin resin, an acrylic resin, or the like can be used.
- As the glass constituting the workpiece quartz glass, sapphire glass, alkali glass, borosilicate glass, or the like can be used.
- Each of the two workpieces may be made of the same material or different materials.
- resin-resin, resin-glass, glass-glass, resin-silicon wafer, glass-silicon wafer, silicon wafer-silicon wafer are preferable.
- a silicon oxide film may be formed on the surface of the silicon wafer.
- the workpiece bonding method of the present invention includes a surface activation step of activating at least one workpiece bonding surface, and a bonding step of bonding two workpieces in a stacked state so that the respective bonding surfaces are in contact with each other. And have.
- the surface activation step only needs to be performed on one of the workpieces, but is preferably performed on both of the two workpieces.
- work bonding method of this invention before performing a surface activation process, the pre-processing process which remove
- the pretreatment process may be performed on the workpiece subjected to the surface activation process. However, when the surface activation process is performed on only one workpiece, the pretreatment process is performed on both of the two workpieces. May be.
- the processing method for executing the pretreatment step is not particularly limited as long as moisture is released from the workpiece bonding surface. Specific examples of this processing method include (1) a method of heating the workpiece, (2) a method of placing the workpiece in a decompression space, and (3) a dry surface or an inert gas with respect to the bonding surface of the workpiece. Examples thereof include a method of spraying a pretreatment gas, and (4) a method of placing a work in a dry atmosphere. Among these, the methods (1), (2) and (3) are preferable.
- FIG. 1 is an explanatory diagram showing an apparatus for performing a pretreatment process by heating a workpiece.
- This apparatus has a hot plate 10 for heating the workpieces W1, W2.
- plate-like workpieces W1 and W2 are placed on a hot plate 10 and directly heated by the hot plate 10.
- the heating conditions for the workpiece W are appropriately set depending on the materials constituting the workpieces W1 and W2, and the heating temperature is preferably 75 ° C. or higher, and more preferably 100 ° C. or higher, which is the boiling point of water.
- the heating temperature is 100 to 110 ° C.
- the heating time is 30 to 300 seconds.
- the heating temperature is 120 to 140 ° C. and the heating time is 30 to 300 seconds.
- FIG. 2 is an explanatory diagram showing an apparatus for performing a pretreatment process by placing a work in a decompression space.
- a stage 21 on which workpieces W1, W2 are placed is provided in a rectangular box-shaped chamber 20.
- a vacuum valve 22 is provided on one side wall 20 a of the chamber 20.
- a leak port 23 is provided on the other side wall 20 b of the chamber 20.
- a vacuum pump 25 is connected to the vacuum valve 22 via a pipe 24.
- the plate-like workpieces W1 and W2 are placed on the stage 21 so that the bonded surfaces face upward. Thereafter, the vacuum pump 25 is driven to make the inside of the chamber 20 a decompressed space.
- the atmospheric pressure in the decompression space in the chamber 20 is, for example, 1000 Pa or less.
- the processing time for placing the workpieces W1, W2 in the decompression space is, for example, 1 to 5 minutes.
- FIG. 3 is an explanatory view showing an apparatus for performing a pretreatment process by spraying a pretreatment gas made of dry air or an inert gas onto a bonding surface of workpieces.
- a pretreatment gas made of dry air or an inert gas onto a bonding surface of workpieces.
- an injection nozzle 35 that injects a pretreatment gas G is disposed above a stage 30 on which workpieces W1 and W2 are placed.
- the dry air constituting the pretreatment gas G it is preferable to use one having a dew point of ⁇ 40 ° C. or less.
- the inert gas constituting the pretreatment gas G nitrogen gas, argon gas, or the like can be used.
- the plate-like workpieces W1 and W2 are placed on the stage 30 so that the bonded surfaces face upward.
- the pretreatment gas G is injected from the injection nozzle 35 and sprayed onto the bonding surfaces of the workpieces W1 and W2.
- the flow rate of the pretreatment gas G sprayed onto the workpieces W1, W2 is preferably 0.03 to 0.12 m 3 / min.
- the processing time during which the pretreatment gas G is blown onto the workpieces W and W2 is, for example, 5 to 300 seconds.
- FIG. 4 is an explanatory diagram showing an apparatus for performing a pretreatment process by placing a workpiece in a dry atmosphere.
- a tray 41 on which workpieces W1 and W2 are placed is provided in a rectangular box-shaped container 40.
- a gas inlet 43 through which dry air is introduced is provided adjacent to one side wall 40a of the container 40.
- the other side wall 40b of the container 40 is provided with a gas discharge port 44 through which the gas in the container 40 is discharged.
- the plate-like workpieces W ⁇ b> 1 and W ⁇ b> 2 are placed on the tray 41 so that the bonded surfaces face upward.
- the tray 41 on which the workpieces W1 and W2 are placed is disposed in the container 40.
- the dry atmosphere in the container 40 preferably has a dew point of ⁇ 20 ° C. or less when the relative humidity is 5% or less, for example, when the processing temperature is room temperature (20 ° C.).
- the degree of the dry atmosphere in the container 40 can be estimated by measuring the dew point of the gas discharged from the gas discharge port 44 with a dew point meter (not shown).
- the processing time for placing the workpieces W1, W2 in a dry atmosphere is, for example, 1 to 5 minutes.
- the mass-based moisture content of the workpiece after completion of the pretreatment step is 0.12% or less.
- the mass-based moisture content can be measured by a heat drying moisture meter.
- the time from the completion of the pretreatment process to the start of the surface activation process is 10 minutes or less.
- this time exceeds 10 minutes, there exists a possibility that a water
- the surface activation process may be an ultraviolet irradiation process for irradiating the workpiece bonding surface with vacuum ultraviolet radiation, or a plasma gas processing process for bringing a process gas that has been made plasma by atmospheric pressure plasma into contact with the workpiece bonding surface. preferable.
- a vacuum ultraviolet ray having a wavelength of 200 nm or less is irradiated on the bonding surface of the pretreated workpiece.
- an excimer lamp such as a xenon excimer lamp having an emission line at a wavelength of 172 nm, a low-pressure mercury lamp having an emission line at a wavelength of 185 nm, or a deuterium lamp having an emission line in the wavelength range of 120 to 200 nm is preferably used. be able to.
- the illuminance of the vacuum ultraviolet rays applied to the workpiece bonding surface is, for example, 10 to 100 mW / cm 2 . Further, the ultraviolet irradiation time for the workpiece bonding surface is appropriately set according to the material constituting the workpiece, and is, for example, 5 to 120 seconds.
- FIG. 5 is a cross-sectional view illustrating the configuration of an example of an atmospheric pressure plasma apparatus used in the present invention.
- This atmospheric pressure plasma apparatus has a rectangular parallelepiped casing 50 made of, for example, aluminum.
- a plate-like electrode 51 electrically connected to a high frequency power supply 55 is disposed horizontally.
- a dielectric layer 52 is formed on the lower surface of the electrode 51.
- the electrode 51 is a high voltage side electrode
- the casing 50 is a ground side electrode.
- a gas supply port 53 for supplying process gas into the casing 50 is provided on the upper surface of the casing 50.
- a plurality of nozzles 54 are formed on the lower surface of the casing 50 to discharge process gas that has been plasmatized by atmospheric pressure plasma in the casing 50 to the outside.
- the process gas G1 is supplied from the gas supply port 53 into the casing 50 under atmospheric pressure or a pressure in the vicinity thereof.
- a high-frequency electric field is applied between the electrode 51 and the casing 50 via the dielectric layer 52 by the high-frequency power supply 55
- a dielectric barrier discharge is generated between the electrode 51 and the casing 50.
- the process gas G1 existing between the casing 50 and the dielectric layer 52 is ionized or excited to be turned into plasma.
- the plasma-processed process gas G ⁇ b> 2 is discharged to the outside from the nozzle 54 of the casing 50 and comes into contact with a bonding surface of a work (not shown) disposed below the casing 50.
- the process gas G1 containing nitrogen gas, argon gas or the like as a main component and containing 0.01 to 5% by volume of oxygen gas.
- a mixed gas of nitrogen gas and clean dry air (CDA) can be used.
- the power supplied from the high frequency power supply 55 has a frequency of 20 to 70 kHz and a voltage of 5 to 15 kVp-p. Further, the processing time by the plasma gas processing is, for example, 5 to 100 seconds.
- joining process In the joining step, the two workpieces are joined in a stacked state so that their bonding surfaces are in contact with each other.
- Specific methods for joining the workpieces include (1) a method of heating in a state in which two workpieces are laminated, (2) a method of pressing in the thickness direction in a state of laminating two workpieces, (3) Examples include a method of heating while pressing in the thickness direction in a state where two workpieces are stacked, and a method of heating after pressing in the thickness direction in a state where two workpieces are stacked and releasing the pressurization.
- Specific conditions in the joining process are appropriately set within a range in which the workpieces are not deformed, depending on the material constituting the workpieces.
- specific heating conditions when two workpieces are heated, when one workpiece is made of a synthetic resin, the heating temperature is 100 to 110 ° C. When both of the two workpieces are made of glass, silicon wafer, crystal or sapphire, the heating temperature is 120 to 140 ° C.
- the applied pressure is 0.2 to 10 MPa. Further, when both the two workpieces are made of glass, silicon wafer, crystal or sapphire, the applied pressure is 1 to 10 MPa.
- the following work A and work B were prepared.
- the workpiece A is made of a cycloolefin resin (“Zeonex 480R” manufactured by Nippon Zeon Co., Ltd.) and has a rectangular plate shape with dimensions of 30 mm ⁇ 30 mm ⁇ 3 mm.
- the workpiece B is made of synthetic quartz glass and has a rectangular plate shape with dimensions of 25 mm ⁇ 45 mm ⁇ 2 mm.
- the mass-based moisture content of each of the workpiece A and workpiece B was measured by a heat drying moisture meter (manufactured by A & D Co.).
- This heat-drying moisture meter heats the sample placed on the electronic balance in the moisture meter, measures the change in the sample mass with the balance, and determines the decrease in the sample mass before and after the heat-drying as moisture. .
- the mass reference moisture content of the workpiece A was 0.13%
- the mass reference moisture content of the workpiece B was 0.07%.
- Example 1 Using workpiece A as one workpiece and workpiece B as the other workpiece, the two workpieces were bonded together by performing the following pretreatment step, ultraviolet irradiation treatment step, and bonding step.
- Pretreatment process Using the apparatus shown in FIG. 1, a pretreatment process was performed by heating each of the two workpieces under the conditions of a heating temperature of 75 ° C. and a heating time of 5 minutes. The mass-based moisture content of each of the workpiece A and workpiece B after the pretreatment step was measured by a heat drying moisture meter (manufactured by A & D). The results are shown in Table 1.
- Example 2 In the pretreatment step, the two workpieces were bonded together in the same manner as in Example 1 except that the heating temperature was changed to 100 ° C. Table 1 shows the mass-based moisture content of each of the two workpieces after the pretreatment step. About the obtained joined body, the tensile shear bond strength was measured based on JISK6850. The results are shown in Table 1.
- Example 3 In the pretreatment step, the two workpieces were bonded in the same manner as in Example 1 except that the heating temperature was changed to 120 ° C. Table 1 shows the mass-based moisture content of each of the two workpieces after the pretreatment step. About the obtained joined body, the tensile shear bond strength was measured based on JISK6850. The results are shown in Table 1.
- Example 4 Two workpieces were bonded together in the same manner as in Example 1 except that the pretreatment step was performed as follows. Table 1 shows the mass-based moisture content of each of the two workpieces after the pretreatment step. About the obtained joined body, the tensile shear bond strength was measured based on JISK6850. The results are shown in Table 1. [Pretreatment process] Using the apparatus shown in FIG. 2, the pretreatment step was performed by placing each of the two workpieces in a reduced pressure space having an atmospheric pressure of 133 Pa for 5 minutes.
- Example 5 Two workpieces were bonded together in the same manner as in Example 1 except that the pretreatment step was performed as follows. Table 1 shows the mass-based moisture content of each of the two workpieces after the pretreatment step. About the obtained joined body, the tensile shear bond strength was measured based on JISK6850. The results are shown in Table 1. [Pretreatment process] Using the apparatus shown in FIG. 3, a pretreatment step was performed by blowing nitrogen gas on one surface (bonding surface) of each of the two workpieces for 5 minutes under the condition that the flow rate was 0.03 m 3 / min. .
- Example 6 Two workpieces were bonded together in the same manner as in Example 1 except that the pretreatment step was performed as follows. Table 1 shows the mass-based moisture content of each of the two workpieces after the pretreatment step. About the obtained joined body, the tensile shear bond strength was measured based on JISK6850. The results are shown in Table 1. [Pretreatment process] Using the apparatus shown in FIG. 4, each of the workpiece A and the workpiece B is placed in a dry atmosphere at a temperature of 20 ° C. and a relative humidity of 5% (dew point is ⁇ 20 ° C.) for 5 minutes to perform a pretreatment process. It was.
- Example 7 The two workpieces were bonded together in the same manner as in Example 1 except that the workpiece A was used instead of the workpiece B as the other workpiece. About the obtained joined body, the tensile shear bond strength was measured based on JISK6850. The results are shown in Table 1.
- Example 8 The two workpieces were bonded together in the same manner as in Example 2 except that the workpiece A was used instead of the workpiece B as the other workpiece. About the obtained joined body, the tensile shear bond strength was measured based on JISK6850. The results are shown in Table 1.
- Example 9 The two workpieces were bonded together in the same manner as in Example 3 except that the workpiece A was used instead of the workpiece B as the other workpiece. About the obtained joined body, the tensile shear bond strength was measured based on JISK6850. The results are shown in Table 1.
- Example 10 The two workpieces were bonded in the same manner as in Example 4 except that workpiece A was used instead of workpiece B as the other workpiece. About the obtained joined body, the tensile shear bond strength was measured based on JISK6850. The results are shown in Table 1.
- Example 11 The two workpieces were bonded together in the same manner as in Example 5 except that workpiece A was used instead of workpiece B as the other workpiece. About the obtained joined body, the tensile shear bond strength was measured based on JISK6850. The results are shown in Table 1.
- Example 12 The two workpieces were bonded together in the same manner as in Example 6 except that the workpiece A was used instead of the workpiece B as the other workpiece. About the obtained joined body, the tensile shear bond strength was measured based on JISK6850. The results are shown in Table 1.
- Example 13 Two workpieces were bonded in the same manner as in Example 1 except that workpiece B was used instead of workpiece A as one workpiece. About the obtained joined body, the tensile shear bond strength was measured based on JISK6850. The results are shown in Table 1.
- Example 14 Two workpieces were bonded together in the same manner as in Example 2 except that workpiece B was used instead of workpiece A as one workpiece. About the obtained joined body, the tensile shear bond strength was measured based on JISK6850. The results are shown in Table 1.
- Example 15 The two workpieces were bonded in the same manner as in Example 3 except that the workpiece B was used instead of the workpiece A as one workpiece. About the obtained joined body, the tensile shear bond strength was measured based on JISK6850. The results are shown in Table 1.
- Example 16 Two workpieces were bonded together in the same manner as in Example 4 except that workpiece B was used instead of workpiece A as one workpiece. About the obtained joined body, the tensile shear bond strength was measured based on JISK6850. The results are shown in Table 1.
- Example 17 The two workpieces were bonded in the same manner as in Example 5 except that the workpiece B was used instead of the workpiece A as one workpiece. About the obtained joined body, the tensile shear bond strength was measured based on JISK6850. The results are shown in Table 1.
- Example 18 Two workpieces were bonded together in the same manner as in Example 6 except that workpiece B was used instead of workpiece A as one workpiece. About the obtained joined body, the tensile shear bond strength was measured based on JISK6850. The results are shown in Table 1.
- Example 19 The two workpieces were bonded in the same manner as in Example 8 except that the following plasma gas treatment step was performed instead of the ultraviolet irradiation treatment step. About the obtained joined body, the tensile shear bond strength was measured based on JISK6850. The results are shown in Table 1.
- Example 20 The two workpieces were bonded in the same manner as in Example 9 except that instead of the ultraviolet irradiation process, a plasma gas treatment process under the same conditions as in Example 19 was performed. About the obtained joined body, the tensile shear bond strength was measured based on JISK6850. The results are shown in Table 1.
- Hot plate 20 Chamber 20a One side wall 20b Other side wall 21
- Stage 22 Vacuum valve 23
- Leak port 24 Pipe 25
- Vacuum pump 30 Stage 35
- Injection nozzle 40 Container 40a One side wall 40b Other side wall 41 Tray 43
- Gas inlet 44 Gas outlet 50
- Electrode 52 Dielectric layer 53
- Gas supply port 54 Nozzle 55 High frequency power supply G
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Abstract
Description
このようなマイクロリアクタを用いた反応分析システムは、マイクロ・トータル・アナリシス・システム(以下、「μTAS」という。)と称されている。このμTASによれば、試薬の体積に対する表面積の比が大きくなることなどから高速かつ高精度の反応分析を行うことが可能となり、また、コンパクトで自動化されたシステムを実現することが可能となる。
接着剤によって貼り合わせる方法においては、接着剤が微小流路に染みだして流路が閉塞したり、微小流路の一部が狭くなって流路の径が不均一となったり、また、流路壁面の均質な特性に乱れが生じたりする、という問題がある。
また、熱融着によって貼り合わせる方法においては、加熱溶融温度以上で融着すると加熱段階で流路がつぶれてしまったり、流路が所定の断面形状に保持されなかったりするため、マイクロチップの高機能化が困難となる、という問題がある。
そこで、近年、例えば真空紫外線を基板の表面に照射することによって、当該基板の表面を活性化させ、その後、基板を貼り合わせる方法が提案されている(特許文献1乃至特許文献5参照。)。また、基板の表面を活性化する方法としては、大気圧またはその近傍下においてプロセスガスをプラズマ化し、このプラズマ化したプロセスガスを基板の表面に接触させる方法を利用することも可能である。
少なくとも一方のワークの貼り合わせ面を活性化する表面活性化工程と、
2つのワークをそれぞれの貼り合わせ面が互いに接触するよう積層した状態で接合する接合工程とを有し、
前記表面活性化工程を行う前に、当該表面活性化工程に供されるワークの貼り合わせ面から水分を離脱させる前処理工程を行うことを特徴とする。
また、前記前処理工程は、前記表面活性化工程に供されるワークを減圧空間に配置することにより行われることが好ましい。
また、前記前処理工程は、前記表面活性化工程に供されるワークの貼り合わせ面に対して、乾燥空気または不活性ガスを吹き付けることにより行われることが好ましい。
また、前記表面活性化工程は、前記ワークの貼り合わせ面に真空紫外線を照射する紫外線照射処理工程であることが好ましい。
また、前記表面活性化工程は、大気圧プラズマによってプラズマ化したプロセスガスを、前記ワークの貼り合わせ面に接触させるプラズマガス処理工程であることが好ましい。
[ワーク]
本発明のワークの貼り合わせ方法は、例えば板状の2つのワーク同士を貼り合わせる方法である。本発明の貼り合わせ方法に適用されるワークは、合成樹脂、ガラス、シリコンウエハ、水晶およびサファイアよりなる群から選ばれる材料よりなるものである。
ワークを構成する合成樹脂としては、ポリジメチルシロキサンなどのシリコーン樹脂、シクロオレフィン樹脂、アクリル樹脂などを用いることができる。
ワークを構成するガラスとしては、石英ガラス、サファイアガラス、アルカリガラス、硼珪酸ガラスなどを用いることができる。
2つのワークの各々は、互いに同種の材料よりなるものであっても異なる材料よりなるものであってもよい。2つのワークの材質の組み合わせとしては、樹脂-樹脂、樹脂-ガラス、ガラス-ガラス、樹脂-シリコンウエハ、ガラス-シリコンウエハ、シリコンウエハ-シリコンウエハが好ましい。なお、シリコンウエハの表面には、シリコン酸化膜が形成されていてもよい。
本発明のワークの貼り合わせ方法は、少なくとも一方のワークの貼り合わせ面を活性化する表面活性化工程と、2つのワークをそれぞれの貼り合わせ面が互いに接触するよう積層した状態で接合する接合工程とを有する。表面活性化工程は、一方のワークのみに対して行われればよいが、2つのワークの両方に対して行われることが好ましい。
そして、本発明のワーク貼り合わせ方法においては、表面活性化工程を行う前に、当該表面活性化工程に供されるワークの貼り合わせ面から水分を離脱させる前処理工程が行われる。
前処理工程は、表面活性化工程に供されるワークに対して行われればよいが、表面活性化工程が一方のワークのみに対して行われる場合においは、2つのワークの両方に対して行ってもよい。
前処理工程を実行するための処理方法としては、ワークの貼り合わせ面から水分を離脱させるものであれば特に限定されない。この処理方法の具体例としては,(1)ワークを加熱する方法、(2)ワークを減圧空間に配置する方法、(3)ワークの貼り合わせ面に対して、乾燥空気または不活性ガスよりなる前処理用ガスを吹き付ける方法、(4)ワークを乾燥雰囲気下に配置する方法などが挙げられる。これらの中では、(1)、(2)および(3)の方法が好ましい。
ワークWの加熱条件は、ワークW1,W2を構成する材料によって適宜設定されるが、加熱温度は、75℃以上であることが好ましく、水の沸点である100℃以上であることがより好ましい。
具体的な加熱条件を挙げると、例えばワークW1またはワークW2が合成樹脂よりなるものである場合には、加熱温度が100~110℃、加熱時間が30~300秒間である。
また、ワークW1およびワークW2がガラス、シリコンウエハ、水晶またはサファイアよりなるものである場合には、加熱温度が120~140℃、加熱時間が30~300秒間である。
図2に示す装置においては、板状のワークW1,W2は、その貼り合わせ面が上方を向くようステージ21上に載置される。その後、真空ポンプ25が駆動されることにより、チャンバー20内が減圧空間とされる。
チャンバー20内の減圧空間の気圧は、例えば1000Pa以下である。
また、ワークW1,W2が減圧空間に配置される処理時間は、例えば1~5分間である。
前処理用ガスGを構成する乾燥空気としては、露点が-40℃以下のものを用いることが好ましい。
また、前処理用ガスGを構成する不活性ガスとしては、窒素ガス、アルゴンガスなどを用いることができる。
図3に示す装置においては、板状のワークW1,W2は、その貼り合わせ面が上方を向くようステージ30上に載置される。その後、前処理用ガスGが噴射ノズル35から噴射され、ワークW1,W2の貼り合わせ面に吹きつけられる。
ワークW1,W2に吹きつけられる前処理用ガスGの流量は、0.03~0.12m3 /minであることが好ましい。
また、ワークW,W2に前処理用ガスGが吹きつけられる処理時間は、例えば5~300秒間である。
図4に示す装置においては、板状のワークW1,W2は、その貼り合わせ面が上方を向くようトレイ41上に載置される。そして、ワークW1,W2が載置されたトレイ41が、容器40内に配置される。その後、乾燥空気がガス導入口43から容器40内に導入されることにより、容器40内が乾燥雰囲気とされる。
容器40内の乾燥雰囲気は、相対湿度が5%以下、例えば処理温度が常温(20℃)であれば、露点が-20℃以下であることが好ましい。容器40内の乾燥雰囲気の程度は、ガス排出口44から排出されるガスの露点を露点計(図示省略)によって測定することにより推定することができる。
また、ワークW1,W2が乾燥雰囲気下に配置される処理時間は、例えば1~5分間である。
ここで、質量基準水分量は、加熱乾燥式水分計によって測定することができる。
表面活性化工程は、ワークの貼り合わせ面に真空紫外線を照射する紫外線照射処理工程、または大気圧プラズマによってプラズマ化したプロセスガスを、ワークの貼り合わせ面に接触させるプラズマガス処理工程であることが好ましい。
表面活性化工程として、紫外線処理工程を選択する場合においては、前処理されたワークの貼り合わせ面に、波長200nm以下の真空紫外線を照射する。
真空紫外線を放射する光源としては、波長172nmに輝線を有するキセノンエキシマランプ等のエキシマランプ、波長185nmに輝線を有する低圧水銀ランプ、波長120~200nmの範囲に輝線を有する重水素ランプを好適に用いることができる。
ワークの貼り合わせ面に照射される真空紫外線の照度は、例えば10~100mW/cm2 である。
また、ワークの貼り合わせ面に対する紫外線の照射時間は、ワークを構成する材料に応じて適宜設定されるが、例えば5~120秒間である。
表面活性化工程として、プラズマガス処理工程を選択する場合においては、大気圧プラズマによってプラズマ化したプロセスガスを、ワークの貼り合わせ面に接触させる。
図5は、本発明に用いられる大気圧プラズマ装置の一例における構成を示す説明用断面図である。この大気圧プラズマ装置は、例えばアルミニウムからなる直方体状のケーシング50を有する。このケーシング50内には、高周波電源55に電気的に接続された板状の電極51が水平に配置されている。この電極51の下面には、誘電体層52が形成されている。この例の大気圧プラズマ装置においては、電極51が高圧側電極とされ、ケーシング50が接地側電極とされている。
ケーシング50の上面には、ケーシング50内にプロセスガスを供給するガス供給口53が設けられている。また、ケーシング50の下面には、ケーシング50内において大気圧プラズマによってプラズマ化したプロセスガスを外部に放出する複数のノズル54が形成されている。
以上において、プロセスガスG1としては、窒素ガス、アルゴンガスなどを主成分とし、酸素ガスが0.01~5体積%含有してなるものを使用することが好ましい。または、窒素ガスとクリーンドライエア(CDA)との混合ガスを用いることも可能である。
また、高周波電源55から供給される電力は、周波数が20~70kHz、電圧が5~15kVp-p である。
また、プラズマガス処理による処理時間は、例えば5~100秒間である。
接合工程においては、2つのワークをそれぞれの貼り合わせ面が互いに接触するよう積層した状態で接合する。
ワーク同士を接合するための具体的な方法としては、(1)2つのワークを積層した状態で加熱する方法、(2)2つのワークを積層した状態で厚み方向に加圧する方法、(3)2つのワークを積層した状態で厚み方向に加圧しながら加熱する方法、(4)2つのワークを積層した状態で厚み方向に加圧し、加圧を解除した後に加熱する方法などが挙げられる。
具体的な加熱条件を挙げると、2つのワークを加熱する場合において、一方のワークが合成樹脂よりなるものであるときには、加熱温度が100~110℃である。また、2つのワークの両方がガラス、シリコンウエハ、水晶またはサファイアよりなるものであるときには、加熱温度が120~140℃である。
また、2つのワークを加圧する場合において、一方のワークが合成樹脂よりなるものであるときには、加圧力が0.2~10MPaである。また、2つのワークの両方がガラス、シリコンウエハ、水晶またはサファイアよりなるものであるときには、加圧力が1~10MPaである。
下記のワークAおよびワークBを作製した。
ワークAは、シクロオレフィン樹脂(日本ゼオン株式会社製「ゼオネックス480R」)よりなり、寸法が30mm×30mm×3mmの矩形の板状のものである。
ワークBは、合成石英ガラスよりなり、寸法が25mm×45mm×2mmの矩形の板状のものである。
ワークAおよびワークBの各々の質量基準水分量を、加熱乾燥式水分計(エー・アンド・ディー社製)によって測定した。この加熱乾燥式水分計は、水分計内にある電子天秤に載せた試料を加熱して、 試料の質量変化を天秤で測定し、加熱乾燥前後の試料質量の減少量を水分として求めるものである。その結果、ワークAの質量基準水分量が0.13%、ワークBの質量基準水分量が0.07%であった。
一方のワークとしてワークAを、他方のワークとしてワークBを用い、2つのワークについて、下記の前処理工程、紫外線照射処理工程および接合工程を行うことによって貼り合わせを行った。
[前処理工程]
図1に示す装置を用い、2つのワークの各々について、加熱温度が75℃、加熱時間が5分間の条件で加熱することによって、前処理工程を行った。前処理工程後におけるワークAおよびワークBの各々の質量基準水分量を、加熱乾燥式水分計(エー・アンド・ディー社製)によって測定した。結果を表1に示す。
[紫外線照射処理工程]
キセノンエキシマランプを用い、2つのワークの各々の一面(貼り合わせ面)に、照度が40mW/cm2 、照射時間が30秒間となる条件で、真空紫外線を照射した。
[接合工程]
2つのワークをそれぞれの一面が互いに接触するよう積層した。ここで、2つのワークの各々の一面における互いに接触する接触面積は625mm2 である。次いで、加圧力が2MPa、加圧時間が300秒間の条件で、加圧することによって、2つのワークを接合した。
得られた接合体について、JIS K 6850に準拠して引張せん断接着強さを測定した。結果を表1に示す。
前処理工程において、加熱温度を100℃に変更したこと以外は実施例1と同様にして、2つのワークの貼り合わせを行った。前処理工程後における2つのワークの各々の質量基準水分量を表1に示す。
得られた接合体について、JIS K 6850に準拠して引張せん断接着強さを測定した。結果を表1に示す。
前処理工程において、加熱温度を120℃に変更したこと以外は実施例1と同様にして、2つのワークの貼り合わせを行った。前処理工程後における2つのワークの各々の質量基準水分量を表1に示す。
得られた接合体について、JIS K 6850に準拠して引張せん断接着強さを測定した。結果を表1に示す。
前処理工程を以下のようにして行ったこと以外は実施例1と同様にして、2つのワークの貼り合わせを行った。前処理工程後における2つのワークの各々の質量基準水分量を表1に示す。
得られた接合体について、JIS K 6850に準拠して引張せん断接着強さを測定した。結果を表1に示す。
[前処理工程]
図2に示す装置を用い、2つのワークの各々を気圧が133Paの減圧空間内に5分間配置することによって、前処理工程を行った。
前処理工程を以下のようにして行ったこと以外は実施例1と同様にして、2つのワークの貼り合わせを行った。前処理工程後における2つのワークの各々の質量基準水分量を表1に示す。
得られた接合体について、JIS K 6850に準拠して引張せん断接着強さを測定した。結果を表1に示す。
[前処理工程]
図3に示す装置を用い、2つのワークの各々の一面(貼り合わせ面)に対し、窒素ガスを流量が0.03m3 /minとなる条件で5分間吹き付けることによって、前処理工程を行った。
前処理工程を以下のようにして行ったこと以外は実施例1と同様にして、2つのワークの貼り合わせを行った。前処理工程後における2つのワークの各々の質量基準水分量を表1に示す。
得られた接合体について、JIS K 6850に準拠して引張せん断接着強さを測定した。結果を表1に示す。
[前処理工程]
図4に示す装置を用い、ワークAおよびワークBの各々を、温度20℃で相対湿度が5%(露点が-20℃)の乾燥雰囲気下に5分間配置することによって、前処理工程を行った。
前処理工程を行わなかったこと以外は実施例1と同様にして、2つのワークの貼り合わせを行った。
得られた接合体について、JIS K 6850に準拠して引張せん断接着強さを測定した。結果を表1に示す。
他方のワークとしてワークBの代わりにワークAを用いたこと以外は実施例1と同様にして、2つのワークの貼り合わせを行った。
得られた接合体について、JIS K 6850に準拠して引張せん断接着強さを測定した。結果を表1に示す。
他方のワークとしてワークBの代わりにワークAを用いたこと以外は実施例2と同様にして、2つのワークの貼り合わせを行った。
得られた接合体について、JIS K 6850に準拠して引張せん断接着強さを測定した。結果を表1に示す。
他方のワークとしてワークBの代わりにワークAを用いたこと以外は実施例3と同様にして、2つのワークの貼り合わせを行った。
得られた接合体について、JIS K 6850に準拠して引張せん断接着強さを測定した。結果を表1に示す。
他方のワークとしてワークBの代わりにワークAを用いたこと以外は実施例4と同様にして、2つのワークの貼り合わせを行った。
得られた接合体について、JIS K 6850に準拠して引張せん断接着強さを測定した。結果を表1に示す。
他方のワークとしてワークBの代わりにワークAを用いたこと以外は実施例5と同様にして、2つのワークの貼り合わせを行った。
得られた接合体について、JIS K 6850に準拠して引張せん断接着強さを測定した。結果を表1に示す。
他方のワークとしてワークBの代わりにワークAを用いたこと以外は実施例6と同様にして、2つのワークの貼り合わせを行った。
得られた接合体について、JIS K 6850に準拠して引張せん断接着強さを測定した。結果を表1に示す。
他方のワークとしてワークBの代わりにワークAを用いたこと以外は比較例1と同様にして、2つのワークの貼り合わせを行った。
得られた接合体について、JIS K 6850に準拠して引張せん断接着強さを測定した。結果を表1に示す。
一方のワークとしてワークAの代わりにワークBを用いたこと以外は実施例1と同様にして、2つのワークの貼り合わせを行った。
得られた接合体について、JIS K 6850に準拠して引張せん断接着強さを測定した。結果を表1に示す。
一方のワークとしてワークAの代わりにワークBを用いたこと以外は実施例2と同様にして、2つのワークの貼り合わせを行った。
得られた接合体について、JIS K 6850に準拠して引張せん断接着強さを測定した。結果を表1に示す。
一方のワークとしてワークAの代わりにワークBを用いたこと以外は実施例3と同様にして、2つのワークの貼り合わせを行った。
得られた接合体について、JIS K 6850に準拠して引張せん断接着強さを測定した。結果を表1に示す。
一方のワークとしてワークAの代わりにワークBを用いたこと以外は実施例4と同様にして、2つのワークの貼り合わせを行った。
得られた接合体について、JIS K 6850に準拠して引張せん断接着強さを測定した。結果を表1に示す。
一方のワークとしてワークAの代わりにワークBを用いたこと以外は実施例5と同様にして、2つのワークの貼り合わせを行った。
得られた接合体について、JIS K 6850に準拠して引張せん断接着強さを測定した。結果を表1に示す。
一方のワークとしてワークAの代わりにワークBを用いたこと以外は実施例6と同様にして、2つのワークの貼り合わせを行った。
得られた接合体について、JIS K 6850に準拠して引張せん断接着強さを測定した。結果を表1に示す。
一方のワークとしてワークAの代わりにワークBを用いたこと以外は比較例1と同様にして、2つのワークの貼り合わせを行った。
得られた接合体について、JIS K 6850に準拠して引張せん断接着強さを測定した。結果を表1に示す。
紫外線照射処理工程の代わりに、以下に示すプラズマガス処理工程を行ったこと以外は実施例8と同様にして、2つのワークの貼り合わせを行った。
得られた接合体について、JIS K 6850に準拠して引張せん断接着強さを測定した。結果を表1に示す。
図5に示す、下記の仕様の大気圧プラズマ装置を用意した。
ケーシングの材質:アルミニウム
電極の材質:表面に溶射によって厚みが500μmのアルミナよりなる皮膜が形成されたスーパーインバー
電極の寸法:50mm×300mm
ケーシングと誘電体層との離間距離:0.5mm
電圧:7.0kVp-p
周波数:60kHz
定格電力:1100VA
上記の大気圧プラズマ装置の下方においてノズルから2mm離間した位置に、ワークをその一面(貼り合わせ面)ガノズルに対向するよう配置した。そして、プロセスガスとして、流量が150L/minの窒素ガスおよび流量が1L/minのクリーンドライエア(プロセスガス中の酸素濃度が約0.14体積%)をケーシング内に供給しながら、大気圧プラズマ装置を作動させることにより、ワークの一面に対して15秒間のプラズマガス処理を行った。
紫外線照射処理工程の代わりに、実施例19と同様の条件のプラズマガス処理工程を行ったこと以外は実施例9と同様にして、2つのワークの貼り合わせを行った。
得られた接合体について、JIS K 6850に準拠して引張せん断接着強さを測定した。結果を表1に示す。
紫外線照射処理工程の代わりに、実施例19と同様の条件のプラズマガス処理工程を行ったこと以外は比較例2と同様にして、2つのワークの貼り合わせを行った。
得られた接合体について、JIS K 6850に準拠して引張せん断接着強さを測定した。結果を表1に示す。
20 チャンバー
20a 一側壁
20b 他側壁
21 ステージ
22 真空バルブ
23 リークポート
24 配管
25 真空ポンブ
30 ステージ
35 噴射ノズル
40 容器
40a 一側壁
40b 他側壁
41 トレイ
43 ガス導入口
44 ガス排出口
50 ケーシング
51 電極
52 誘電体層
53 ガス供給口
54 ノズル
55 高周波電源
G 前処理用ガス
G1 プロセスガス
G2 プラズマ化したプロセスガス
W1,W2 ワーク
Claims (6)
- それぞれ合成樹脂、ガラス、シリコンウエハ、水晶およびサファイアからなる群から選択される材料からなる2つのワーク同士を貼り合わせる方法であって、
少なくとも一方のワークの貼り合わせ面を活性化する表面活性化工程と、
2つのワークをそれぞれの貼り合わせ面が互いに接触するよう積層した状態で接合する接合工程とを有し、
前記表面活性化工程を行う前に、当該表面活性化工程に供されるワークの貼り合わせ面から水分を離脱させる前処理工程を行うことを特徴とするワークの貼り合わせ方法。 - 前記前処理工程は、前記表面活性化工程に供されるワークを加熱することにより行われることを特徴とする請求項1に記載のワークの貼り合わせ方法。
- 前記前処理工程は、前記表面活性化工程に供されるワークを減圧空間に配置することにより行われることを特徴とする請求項1に記載のワークの貼り合わせ方法。
- 前記前処理工程は、前記表面活性化工程に供されるワークの貼り合わせ面に対して、乾燥空気または不活性ガスを吹き付けることにより行われることを特徴とする請求項1に記載のワークの貼り合わせ方法。
- 前記表面活性化工程は、前記ワークの貼り合わせ面に真空紫外線を照射する紫外線照射処理工程であることを特徴とする請求項1乃至請求項4のいずれかに記載のワークの貼り合わせ方法。
- 前記表面活性化工程は、大気圧プラズマによってプラズマ化したプロセスガスを、前記ワークの貼り合わせ面に接触させるプラズマガス処理工程であることを特徴とする請求項1乃至請求項4のいずれかに記載のワークの貼り合わせ方法。
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JP2016554067A JPWO2016060080A1 (ja) | 2014-10-15 | 2015-10-09 | ワークの貼り合わせ方法 |
US15/518,364 US20170305069A1 (en) | 2014-10-15 | 2015-10-09 | Workpiece bonding method |
KR1020177012951A KR20170071539A (ko) | 2014-10-15 | 2015-10-09 | 워크의 붙임 방법 |
EP15850483.7A EP3208070A4 (en) | 2014-10-15 | 2015-10-09 | Workpiece bonding method |
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Cited By (2)
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JP2017193134A (ja) * | 2016-04-22 | 2017-10-26 | 国立大学法人東京工業大学 | 合成樹脂からなる基材の接合方法 |
WO2018012276A1 (ja) * | 2016-07-15 | 2018-01-18 | ウシオ電機株式会社 | 基板の貼り合わせ方法およびマイクロチップの製造方法 |
Families Citing this family (2)
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CN109721257B (zh) * | 2018-08-02 | 2020-06-19 | 比亚迪股份有限公司 | 玻璃复合体、壳体、显示装置以及终端设备 |
CN115028141A (zh) * | 2022-08-11 | 2022-09-09 | 西北电子装备技术研究所(中国电子科技集团公司第二研究所) | 一种蓝宝石压力敏感结构的蓝宝石晶圆直接键合方法 |
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Cited By (7)
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JP2017193134A (ja) * | 2016-04-22 | 2017-10-26 | 国立大学法人東京工業大学 | 合成樹脂からなる基材の接合方法 |
WO2018012276A1 (ja) * | 2016-07-15 | 2018-01-18 | ウシオ電機株式会社 | 基板の貼り合わせ方法およびマイクロチップの製造方法 |
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TWI697407B (zh) * | 2016-07-15 | 2020-07-01 | 日商牛尾電機股份有限公司 | 基板的貼合方法及微晶片的製造方法 |
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JPWO2016060080A1 (ja) | 2017-07-06 |
US20170305069A1 (en) | 2017-10-26 |
KR20170071539A (ko) | 2017-06-23 |
TW201625403A (zh) | 2016-07-16 |
EP3208070A4 (en) | 2018-06-06 |
EP3208070A1 (en) | 2017-08-23 |
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