WO2011046059A1 - Dispositif permettant de détecter une substance dans un liquide et procédé de fabrication associé - Google Patents

Dispositif permettant de détecter une substance dans un liquide et procédé de fabrication associé Download PDF

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Publication number
WO2011046059A1
WO2011046059A1 PCT/JP2010/067626 JP2010067626W WO2011046059A1 WO 2011046059 A1 WO2011046059 A1 WO 2011046059A1 JP 2010067626 W JP2010067626 W JP 2010067626W WO 2011046059 A1 WO2011046059 A1 WO 2011046059A1
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Prior art keywords
substrate
resin layer
wave element
detection device
acoustic wave
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PCT/JP2010/067626
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English (en)
Japanese (ja)
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雅章 安田
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株式会社村田製作所
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Publication of WO2011046059A1 publication Critical patent/WO2011046059A1/fr

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
    • G01N29/02—Analysing fluids
    • G01N29/022—Fluid sensors based on microsensors, e.g. quartz crystal-microbalance [QCM], surface acoustic wave [SAW] devices, tuning forks, cantilevers, flexural plate wave [FPW] devices
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
    • G01N29/22—Details, e.g. general constructional or apparatus details
    • G01N29/222—Constructional or flow details for analysing fluids
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2291/00—Indexing codes associated with group G01N29/00
    • G01N2291/02—Indexing codes associated with the analysed material
    • G01N2291/025—Change of phase or condition
    • G01N2291/0255—(Bio)chemical reactions, e.g. on biosensors
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2291/00—Indexing codes associated with group G01N29/00
    • G01N2291/02—Indexing codes associated with the analysed material
    • G01N2291/025—Change of phase or condition
    • G01N2291/0256—Adsorption, desorption, surface mass change, e.g. on biosensors
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2291/00—Indexing codes associated with group G01N29/00
    • G01N2291/04—Wave modes and trajectories
    • G01N2291/042—Wave modes
    • G01N2291/0423—Surface waves, e.g. Rayleigh waves, Love waves

Definitions

  • the present invention relates to a manufacturing method of a submerged substance detection device and a submerged substance detection device, and more particularly to a manufacturing method of a submerged substance detection device including a surface acoustic wave element and a submerged substance detection device.
  • Patent Document 1 proposes an in-liquid substance detection apparatus using a surface acoustic wave element as an example of an in-liquid substance detection apparatus.
  • FIG. 15 is a partially cutaway enlarged front cross-sectional view in which a main part of the in-liquid substance detection device described in Patent Document 1 is enlarged.
  • the in-liquid substance detection device 100 has a base substrate 101 in which an opening 101c is formed.
  • a protective member 103 is disposed on the surface of one side of the base substrate 101 with an adhesion layer 102 interposed therebetween.
  • An opening 103a is formed in the protection member 103, and the opening 103a is connected to the opening 101c.
  • a protective member 104 is disposed on the other surface of the base substrate 101.
  • An opening 104a is formed in the protection member 104, and the opening 104a is connected to the opening 101c.
  • a surface acoustic wave element 105 is disposed in the opening 104a.
  • the surface acoustic wave element 105 includes a piezoelectric substrate 105a.
  • An IDT electrode 105b is formed on the surface 105a1 of the piezoelectric substrate 105a.
  • the IDT electrode 105b is covered with a reaction film 105c to which a detection target substance in the liquid binds.
  • the surface acoustic wave element 105 is mounted on electrode lands 101a and 101b provided on the other surface of the base substrate 101 via bump electrodes 106a and 106b. Note that the joint portion formed by the bump electrodes 106 a and 106 b is sealed with a resin layer 107.
  • the in-liquid substance detection device 100 when the liquid containing the detection target substance adheres to the sensing unit 110 of the surface acoustic wave element 105 provided with the IDT electrode 105b and the reaction film 105c via the openings 103a and 101c, The detection target substance is bonded to the reaction film 105c. For this reason, the load applied to the IDT electrode 105b of the surface acoustic wave element 105 varies. Therefore, the output from the surface acoustic wave element 105 fluctuates, and the presence or absence of the detection target substance and the concentration of the detection target substance are detected based on the change in the output value.
  • the detection target substance can be detected even when the amount of the liquid containing the detection target substance is small. It is very useful for detecting substances in the biotechnology field where trace amounts are used.
  • the substance detection results may vary. That is, the submerged substance detection device 100 may not be able to detect the substance stably with high accuracy.
  • the present invention has been made in view of such a point, and an object of the present invention is to provide a method for manufacturing a submerged substance detection apparatus and a submerged substance detection apparatus capable of stably detecting a substance with high accuracy. is there.
  • the present inventors have found that the bleed generated from the resin layer 107 may cause a variation in the detection result of the substance when the substance is detected using the submerged substance detection apparatus 100. I found out. That is, when the bleed generated from the resin layer 107 adheres to the sensing unit 110, elutes in the liquid, or swells, the load applied to the sensing unit 110 varies regardless of the presence or absence of the detection target substance. It has been found that the detection results of substances may vary, and as a result, the present invention has been made.
  • the method for manufacturing a submerged substance detection device includes a substrate having an opening, a piezoelectric substrate, and an IDT electrode that is formed on the piezoelectric substrate and forms a sensing unit. And a surface acoustic wave device mounted on the substrate so that the sensing portion faces the opening of the substrate, and a resin layer formed so as to surround the sensing portion between the substrate and the surface acoustic wave element.
  • the present invention relates to a method for manufacturing a submerged substance detection device, in which a detection concave portion in which a liquid to be detected is stored is formed by an opening of a substrate and a resin layer.
  • the method for manufacturing a submerged substance detection device includes a preparation step of preparing a mounting structure in which the surface acoustic wave element is mounted on a substrate having at least an inner surface of an opening that is hydrophobic, A resin layer forming step of forming a resin layer so as to surround the sensing portion between the surface acoustic wave element and a hydrophilic step of applying a hydrophilic treatment to the surface of the detection concave portion are provided.
  • the mounting structure includes an annular wall portion so as to surround the sensing portion, and the resin layer is walled in the resin layer forming step. It forms outside the part. In this case, since the bleed from the resin layer enters the concave portion for detection by the wall portion, it is possible to manufacture an in-liquid substance detection device with higher detection accuracy.
  • the preparation step includes a step of mounting the surface acoustic wave element on the substrate, and an inner surface of the opening of the substrate on which the surface acoustic wave element is mounted. And hydrophobizing treatment.
  • the degree of freedom in designing the substrate can be increased.
  • the preparation step includes a step of subjecting the inner surface of the opening of the substrate to a hydrophobic treatment, and a substrate having the inner surface of the opening subjected to the hydrophobic treatment. And mounting a surface acoustic wave device on the substrate.
  • a hydrophobic substance since it is not always necessary to include a hydrophobic substance in the substrate, the degree of freedom in designing the substrate can be increased.
  • the hydrophobic treatment on the inner surface of the opening is performed by discharging a hydrophobic treatment agent from a nozzle inserted in the opening.
  • the substrate includes a hydrophobic substance.
  • a hydrophobic treatment it is not always necessary to apply a hydrophobic treatment to the inner surface of the opening of the substrate. Therefore, the manufacturing process of the submerged substance detection device can be simplified.
  • the resin layer is formed by placing a thermosetting resin and curing the thermosetting resin by heating.
  • a thermosetting resin is used, bleed is likely to occur even when the resin is cured.
  • the thermosetting resin is used. Even so, it is possible to manufacture a substance detection apparatus with high detection accuracy.
  • the resin layer forming step is performed so that the resin layer is not positioned in the opening when viewed from the opening direction of the opening of the substrate. It is a process of forming a layer. In this case, since it can suppress more effectively that a bleed enters in the recessed part for a detection, the submerged substance detection apparatus with a higher detection precision can be manufactured.
  • the hydrophilization step is performed by performing plasma treatment or UV treatment on the surface of the detection recess.
  • the submerged substance detection device includes a substrate, a surface acoustic wave element, and a resin layer.
  • An opening is formed in the substrate.
  • the surface acoustic wave element has a piezoelectric substrate and an IDT electrode.
  • the IDT electrode is formed on the piezoelectric substrate.
  • the IDT electrode constitutes a sensing unit.
  • the surface acoustic wave element is mounted on the substrate so that the sensing unit faces the opening of the substrate.
  • the resin layer is formed outside the sensing unit between the substrate and the surface acoustic wave element.
  • a detection recess for storing a liquid to be detected is formed by the opening of the substrate and the resin layer.
  • the wall surface of the detection recess is hydrophilic.
  • the submerged substance detection device further includes a hydrophobic layer.
  • the hydrophobic layer is positioned closer to the detection recess than the resin layer on the surface of the substrate on the surface acoustic wave element side, and positioned closer to the detection recess than the resin layer on the substrate side of the surface acoustic wave element. It is formed on at least one of the portions.
  • the hydrophobic layer is formed on at least a portion located on the detection recess side of the resin layer on the surface of the substrate on the surface acoustic wave element side. Has been.
  • the hydrophobic layer includes a portion located on the detection recess side of the resin layer on the surface of the substrate on the surface acoustic wave element side, and a surface acoustic wave. It is formed on both the resin layer on the substrate side surface of the element and the portion located on the detection recess side.
  • the hydrophobic layer is formed in an annular shape so as to surround the detection recess.
  • the resin layer is formed in an annular shape so as to surround the detection recess.
  • the hydrophobic layer and the resin layer are formed concentrically so as to surround the detection recess.
  • the gap between the substrate and the surface acoustic wave element is formed by the hydrophobic layer of the gap due to the water repellency of the hydrophobic layer. This is the distance at which the liquid to be detected supplied to the detection concave portion is prevented from entering the portion where the detection is performed.
  • the gap between the substrate and the surface acoustic wave element in the region where the hydrophobic layer is formed is 100 ⁇ m or less.
  • the submerged substance detection device is arranged so as to reach the surface acoustic wave element from the substrate in a portion located on the detection recess side of the resin layer. A wall portion formed is further provided.
  • the resin layer is formed in a state where the inner surface of the opening of the substrate is hydrophobic, it is possible to prevent the bleed generated from the resin layer from entering the detection recess. Is done. Therefore, according to the manufacturing method of the present invention, it is possible to manufacture an in-liquid substance detection device capable of detecting a substance with high accuracy and stability.
  • the submerged substance detection device includes a portion located on the detection recess side of the surface of the surface acoustic wave element side of the substrate and a resin layer on the surface of the surface acoustic wave element on the substrate side. Is also provided with a hydrophobic layer formed on at least one of the portions located on the detection recess side. For this reason, the liquid to be detected reaches the resin layer effectively by the water repellency of the hydrophobic layer. For this reason, the fall of the detection accuracy resulting from the elution of the bleed at the time of a detection can be suppressed effectively. In addition, since the wall surface of the detection recess is hydrophilic, the detection liquid can be stably taken in and out and replaced.
  • FIG. 1 is a schematic plan view of the submerged substance detection device according to the first embodiment.
  • FIG. 2 is a schematic cross-sectional view taken along the line II-II in FIG.
  • FIG. 3 is a schematic cross-sectional view taken along line III-III in FIG. 4 is a schematic cross-sectional view taken along line VI-VI in FIG.
  • FIG. 5 is a schematic plan view of the substrate.
  • FIG. 6 is a schematic configuration diagram of the sensing unit.
  • FIG. 7 is a flowchart showing a manufacturing process of the submerged substance detection device according to the first embodiment.
  • FIG. 8 is a schematic cross-sectional view showing the hydrophobization process.
  • FIG. 9 is a schematic cross-sectional view of the in-liquid substance detection device of the second embodiment.
  • FIG. 10 is a flowchart showing a manufacturing process of the submerged substance detection device according to the second embodiment.
  • FIG. 11 is a schematic cross-sectional view of the in-liquid substance detection device of the third embodiment.
  • FIG. 12 is a graph showing the amount of frequency change in the example.
  • FIG. 13 is a graph showing the frequency change amount in the comparative example.
  • FIG. 14 is a schematic configuration diagram of a sensing unit in a modified example.
  • FIG. 15 is a partially cutaway enlarged front cross-sectional view in which a main part of the in-liquid substance detection device described in Patent Document 1 is enlarged.
  • FIG. 16 is a schematic cross-sectional view of the submerged substance detection device of the fourth embodiment.
  • FIG. 17 is a schematic cross-sectional view of the in-liquid substance detection device of the fifth embodiment.
  • FIG. 18 is a schematic cross-sectional view of the in-liquid substance detection device of the sixth embodiment.
  • FIG. 19 is a schematic plan view of the in-liquid substance detection device of the seventh embodiment.
  • FIG. 20 is a schematic plan view of the submerged substance detection device according to the eighth embodiment.
  • FIG. 21 is a schematic plan view of the submerged substance detection device of the ninth embodiment.
  • FIG. 1 is a schematic plan view of a submerged substance detection device 1 of the present embodiment
  • FIGS. 2 to 4 are schematic cross-sectional views of the submerged substance detection device 1.
  • FIG. 1 and the like the IDT electrode is represented by a rectangle with two diagonal lines drawn.
  • FIG. 1 etc. the drawing of a reflector is abbreviate
  • the number of electrode fingers is smaller than the actual number.
  • the in-liquid substance detection device 1 is an apparatus for detecting a substance present in the liquid. By using the in-liquid substance detection device 1, the concentration of the substance present in the liquid can be measured. Examples of the liquid to be detected include a dispersion solution in which an aqueous solution or a colloid is dispersed.
  • the submerged substance detection device 1 includes a surface acoustic wave element (SAW element) 10 and a substrate 30.
  • the surface acoustic wave element 10 includes a piezoelectric substrate 11.
  • the piezoelectric substrate 11 is not particularly limited.
  • the piezoelectric substrate 11 can be configured by a piezoelectric single crystal substrate such as a LiNbO 3 substrate or a LiTaO 3 substrate, a piezoelectric ceramic substrate, or the like.
  • First and second IDT electrodes 12 and 15 are formed on the piezoelectric substrate 11.
  • the first and second IDT electrodes 12 and 15 constitute first and second sensing units 18 and 19 that detect substances in the liquid, respectively.
  • the first IDT electrode 12 has two pairs of comb electrodes 12a, 12b, 12c, and 12d that are interleaved with each other.
  • the comb electrode 12a is connected to the first input / output port 12e.
  • the comb electrode 12c is connected to the second input / output port 12g, and the comb electrode 12b is connected to the ground port 12f.
  • the comb electrode 12d is connected to the ground port 12h.
  • Grating reflectors 13 and 14 are disposed on both sides in the elastic wave propagation direction of the region where the first IDT electrode 12 is provided.
  • the second IDT electrode 15 also has two pairs of comb electrodes 15a, 15b, 15c, and 15d that are inserted into each other in the same manner as the first IDT electrode 12.
  • the comb electrode 15b is connected to the first input / output port 15f.
  • the comb electrode 15d is connected to the second input / output port 15h, and the comb electrode 15a is connected to the ground port 15e.
  • the comb electrode 15c is connected to the ground port 15g.
  • Grating reflectors 16 and 17 are disposed on both sides of the region where the second IDT electrode 15 is provided in the elastic wave propagation direction.
  • bump electrodes 21a, 21b, 21c, 21d, 22a, 22b, 22c, and 22d are formed on the piezoelectric substrate 10.
  • bump electrodes 21c, 21d, 22c, and 22d are bump electrodes that are connected to the ground electrode
  • bump electrodes 21a, 21b, 22a, and 22b are bump electrodes that are connected to the input / output ports.
  • the bump electrode 21a is connected to the first input / output port 12e.
  • the bump electrode 21b is connected to the second input / output port 12g.
  • the bump electrode 21c is connected to the ground port 12f.
  • the bump electrode 21d is connected to the ground port 12h.
  • the bump electrode 22a is connected to the first input / output port 15f.
  • the bump electrode 22b is connected to the second input / output port 15h.
  • the bump electrode 22c is connected to the ground port 15e.
  • the bump electrode 22d is connected to the ground port 15g.
  • the first and second IDT electrodes are formed by two pairs of interdigital electrodes interleaved with each other.
  • the second IDT electrode may be formed by a pair of comb electrodes interleaved with each other.
  • impedance matching with the circuit connected to the surface acoustic wave element 10 tends to be difficult as compared with the case where two pairs of comb-tooth electrodes are formed, but the submerged substance detection device 1 has a simpler configuration. Since this can be realized, it is easier to reduce the size of the apparatus.
  • each of the bump electrodes 21 a, 21 b, 21 c, 21 d, 22 a, 22 b, 22 c, 22 d is exposed from the protective film 20 described later and is higher than the surface of the protective film 20. Projects to the position.
  • Each of the first and second IDT electrodes 12 and 15, grating reflectors 13, 14, 16, 17 and bump electrodes 21a, 21b, 21c, 21d, 22a, 22b, 22c, and 22d is, for example, Ag, It can be formed of an appropriate conductive material such as a metal such as Au, Pd, Pt, Al, Cu, and Ti, or an alloy such as Ag—Pd.
  • Each of the first and second IDT electrodes 12, 15, grating reflectors 13, 14, 16, 17, and bump electrodes 21a, 21b, 21c, 21d, 22a, 22b, 22c, 22d includes a plurality of conductive layers. May be constituted by a conductive layer laminate in which is laminated.
  • a protective film 20 is formed on the piezoelectric substrate 10.
  • the protective film 20 covers the first and second IDT electrodes 12 and 15 and the grating reflectors 13, 14, 16 and 17.
  • the protective film 20 is a layer for protecting the first and second IDT electrodes 12 and 15 and the grating reflectors 13, 14, 16, and 17 from liquids, dust, and the like.
  • the protective film 20 can be formed of an insulating material such as silicon oxide such as SiO 2 or silicon nitride such as SiN.
  • reaction film is a film that reacts with a substance in a liquid.
  • adsorption film is a film that adsorbs a substance in the liquid.
  • a substrate 30 is disposed on the surface acoustic wave element 10.
  • This substrate 30 is for forming a detection recess for storing the liquid to be detected on the upper portions of the sensing units 18 and 19.
  • the substrate 30 is formed with first and second openings 30a and 30b. These openings 30 a and 30 b are formed larger than the sensing portions 18 and 19.
  • the surface acoustic wave element 10 is mounted on the substrate 30 so that the openings 30 a and 30 b of the substrate 30 face the sensing units 18 and 19.
  • the substrate 30 is not particularly limited as long as the substrate 30 has rigidity capable of supporting the surface acoustic wave element 10.
  • the substrate 30 may be a substrate made of an inorganic material, a substrate made of an organic material, or a substrate containing both an inorganic material and an organic material.
  • the substrate 30 can be composed of, for example, a glass epoxy substrate, a glass substrate, a ceramic substrate, a resin substrate, or the like.
  • substrate 30 may be comprised with the film.
  • the glass epoxy substrate is a substrate formed by immersing an epoxy resin in a glass woven fabric in which glass fibers are knitted into a cloth shape.
  • a conductive layer 31 is formed on the substrate 30.
  • the conductive layer 31 includes not only the surface 30 c of the substrate 30 on the surface acoustic wave element 10 side, but also the inner surfaces of the first and second openings 30 a and 30 b and the surface acoustic wave element 10 of the substrate 30.
  • the back surface 30d opposite to the side is covered. Thereby, the deterioration by the corrosion of the board
  • substrate 30 is suppressed.
  • the conductive layer 31 includes a layer having excellent corrosion resistance such as an Au layer, deterioration of the substrate 30 due to corrosion can be more effectively suppressed.
  • deterioration due to corrosion of the substrate 30 is particularly likely to proceed on the inner surfaces of the first and second openings 30a and 30b that are in contact with the liquid, and therefore, the back surface 30d of the substrate 30 and the first and second openings 30a and 30b are not affected. It is preferable to form the conductive layer 31 on the inner surfaces, particularly on the inner surfaces of the first and second openings 30a and 30b.
  • the portion located on the surface 30c of the conductive layer 31 constitutes a ground electrode 31a and first to fourth electrode lands 31b to 31e.
  • the bump electrode 21a is connected to the first electrode land 31b
  • the bump electrode 21b is connected to the second electrode land 31c
  • the bump electrode 22a is connected to the third electrode land 31d.
  • the electrode 22b is connected to the fourth electrode land 31e
  • the bump electrodes 21c, 21d, 22c, and 22d are mounted on the substrate 30 so as to be connected to the ground electrode 31a.
  • a resin layer 40 is disposed between the substrate 30 and the surface acoustic wave element 10.
  • the resin layer 40 is connected to the surface 30 c of the substrate 30 and the surface of the surface acoustic wave element 10. Specifically, the resin layer 40 bonds the substrate 30 and the surface acoustic wave element 10 together.
  • the resin layer 40 is formed so as to surround the sensing units 18 and 19. That is, in the present embodiment, the resin layer 40 is formed in a portion other than the top of the sensing units 18 and 19.
  • the resin layer 40 and the first and second openings 30 a and 30 b formed in the substrate 30 form first and second detection recesses 32 and 33.
  • the resin layer 40 is formed so as not to be positioned in the openings 30 a and 30 b when viewed from the opening direction x of the openings 30 a and 30 b of the substrate 30. That is, the edge part of the resin layer 40 is located outside the openings 30a and 30b.
  • the resin layer 40 is particularly limited as long as it can adhere the substrate 30 and the surface acoustic wave element 10 and has a certain degree of durability against the liquid supplied to the detection recesses 32 and 33.
  • the resin layer 40 may be, for example, a thermoplastic resin or an energy ray curable resin that is cured by energy rays.
  • the energy rays include heat rays and light rays.
  • the energy ray curable resin includes a thermosetting resin, a photocurable resin, and the like.
  • the resin layer 40 can be formed of, for example, an epoxy resin or a polyimide resin.
  • a surface acoustic wave element 10 and a substrate 30 are prepared in step S1.
  • step S2 the surface acoustic wave element 10 is flip-chip mounted on the substrate 30, whereby the ground electrode 31a, the first to fourth electrode lands 31b to 31e, and the bump electrodes 21a, 21b, 22a, 22b, 21c. , 21d, 22c, and 22d.
  • the mounting of the surface acoustic wave element 10 on the substrate 30 is not limited to flip chip mounting.
  • the surface acoustic wave element 10 may be mounted on the substrate 30 by a mounting method other than flip chip mounting.
  • a hydrophobic treatment is performed. Specifically, at least the inner surfaces of the first and second openings 30a and 30b are subjected to a hydrophobic treatment. Specifically, in the present embodiment, the first and second openings 30a and 30b, the portion of the surface 30c of the substrate 30 located near the first and second openings 30a and 30b, and the first and second openings The surface of the two sensing units 18 and 19 is subjected to a hydrophobic treatment.
  • the method of the hydrophobic treatment is not particularly limited, and for example, the hydrophobic treatment can be performed by applying a hydrophobic treatment agent on the surface.
  • a hydrophobic treatment agent on the surface.
  • the nozzle 41 is inserted into the openings 30a and 30b, and the hydrophobic treatment agent is discharged from the nozzle 41, whereby the hydrophobic treatment agent is applied to the surface. Apply. Thereafter, the surface is washed with a washing liquid and dried to complete the hydrophobization treatment.
  • the hydrophobizing agent include bleed inhibitors such as non-bleed N-11 and non-bleed N-31.
  • a mounting structure 42 (see FIG. 7) is prepared in which the surface acoustic wave element 10 is mounted on the substrate 30 in which at least the inner surfaces of the openings 30a and 30b are hydrophobic.
  • step S4 resin layer forming step shown in FIG. 7, the resin layer 40 is formed, and the detection recesses 32 and 33 are formed. Specifically, a nozzle is set between the substrate 30 and the surface acoustic wave element 10, and sealing resin (underfill) is discharged from the nozzle. The discharged resin enters the back of the gap by capillary action. Thereafter, the resin layer 40 is formed by curing the resin. The resin is cured by, for example, supplying heat when the resin is a thermosetting resin and supplying light when the resin is a photocurable resin.
  • the injection of the resin into the gap between the substrate 30 and the surface acoustic wave element 10 is performed so that the resin is not located in the openings 30a and 30b when viewed from the opening direction of the openings 30a and 30b. It is preferable. That is, it is preferable to form the resin layer 40 so that the resin layer 40 is not located in the openings 30a and 30b when viewed from the opening direction of the openings 30a and 30b.
  • step S5 the surface of the detection recesses 32 and 33 is subjected to a hydrophilic treatment.
  • a hydrophilic treatment is not specifically limited, For example, you may perform a hydrophilic treatment by apply
  • the surfaces of the first and second openings 30a and 30b and the sensing portions 18 and 19 are subjected to a hydrophobic treatment. For this reason, the bleed generated during resin filling or curing is repelled by the hydrophobized surface and hardly flows into the detection recesses 32 and 33. Therefore, the bleed is less likely to adhere to the sensing units 18 and 19.
  • the amount of bleed existing in the detection recesses 32 and 33 can be reduced, characteristic changes of the sensing units 18 and 19 due to bleed eluting into the liquid or bleed swell during detection, It is possible to suppress a decrease in measurement accuracy due to a change in liquid characteristics. Therefore, the substance in the liquid can be detected stably with high measurement accuracy.
  • the resin layer 40 is not located in the openings 30a and 30b. Therefore, it is possible to more effectively suppress the bleed from entering the detection recesses 32 and 33.
  • the generated bleed is generally a low viscosity component contained in the resin, typically a low molecular weight component.
  • Specific examples of the bleed include additives such as a curing agent and uncured resin.
  • the present invention is not limited to this.
  • at least the substrate 30 of the substrate 30 and the surface acoustic wave element 10 may be subjected to a hydrophobic treatment.
  • the substrate 30 may be a substrate having a hydrophobic surface.
  • the substrate 30 may include a hydrophobic substance. In that case, it is not always necessary to perform the hydrophobization treatment.
  • the hydrophobic substance include polytetrafluoroethylene (PTFE) and fluororesin.
  • the submerged substance detection device 2 of the present embodiment shown in FIG. 9 is substantially the same as the submerged substance detection device 1 of the first embodiment except that the submerged substance detection device 2 has first and second wall portions 43 and 44. It has the composition of. As shown in FIG. 9, in the present embodiment, the surface of the piezoelectric substrate 11 is formed in an annular shape so as to surround the sensing portions 18 and 19, and the first and second walls extending toward the substrate 30 side. Portions 43 and 44 are formed. The resin layer 40 is located outside the first and second wall portions 43 and 44.
  • tips of the first and second wall portions 43 and 44 may reach the substrate 30 or may not reach the substrate 30.
  • step S11 the surface acoustic wave element 10 and the substrate 30 are prepared as in step S1 described above.
  • step S12 the substrate 30 is hydrophobized.
  • This hydrophobizing process is the same as the hydrophobizing process described in the first embodiment. However, when the substrate 30 includes a hydrophobic substance, step S12 is not necessarily performed.
  • step S13 the surface acoustic wave element 10 is mounted on the substrate 30 as in step S2.
  • step S14 the resin layer 40 is formed in the same manner as in step S4.
  • step S ⁇ b> 14 the resin layer 40 is formed outside the wall portions 43 and 44. That is, the resin is prevented from entering the walls 43 and 44.
  • step S15 a hydrophilic treatment is performed in the same manner as in step S5.
  • step S12 since the hydrophobization process is performed in step S12, it is possible to prevent the bleed from entering the detection recesses 32 and 33. Moreover, since the wall parts 43 and 44 are provided, it can suppress more effectively that a bleed enters the recessed parts 32 and 33 for a detection. Therefore, it is possible to more effectively suppress a decrease in detection accuracy due to bleeding.
  • the wall portions 43 and 44 are formed on the piezoelectric substrate 11 .
  • the present invention is not limited to this configuration.
  • the wall portions 43 and 44 may be formed on the substrate 30.
  • FIG. 16 is a schematic cross-sectional view of the submerged substance detection device of the fourth embodiment.
  • FIG. 6 is referred to in common with the first embodiment.
  • the 16 is a device for detecting substances present in the liquid to be detected.
  • the concentration of the substance present in the liquid to be detected can be measured.
  • the submerged substance detection device 4 includes a surface acoustic wave element (SAW element) 10 and a substrate 30.
  • the surface acoustic wave element 10 includes a piezoelectric substrate 11.
  • the piezoelectric substrate 11 is not particularly limited.
  • the piezoelectric substrate 11 can be configured by a piezoelectric single crystal substrate such as a LiNbO 3 substrate or a LiTaO 3 substrate, a piezoelectric ceramic substrate, or the like.
  • First and second IDT electrodes 12 and 15 are formed on the piezoelectric substrate 11.
  • the first and second IDT electrodes 12 and 15 constitute first and second sensing units 18 and 19 that detect substances in the liquid, respectively.
  • the first IDT electrode 12 has two pairs of comb electrodes 12a, 12b, 12c, and 12d that are interleaved with each other.
  • the comb electrode 12a is connected to the first input / output port 12e.
  • the comb electrode 12c is connected to the second input / output port 12g, and the comb electrode 12b is connected to the ground port 12f.
  • the comb electrode 12d is connected to the ground port 12h.
  • Grating reflectors 13 and 14 are disposed on both sides in the elastic wave propagation direction of the region where the first IDT electrode 12 is provided.
  • the second IDT electrode 15 also has two pairs of comb electrodes 15a, 15b, 15c, and 15d that are inserted into each other in the same manner as the first IDT electrode 12.
  • the comb electrode 15b is connected to the first input / output port 15f.
  • the comb electrode 15d is connected to the second input / output port 15h, and the comb electrode 15a is connected to the ground port 15e.
  • the comb electrode 15c is connected to the ground port 15g.
  • Grating reflectors 16 and 17 are disposed on both sides of the region where the second IDT electrode 15 is provided in the elastic wave propagation direction.
  • the first and second IDT electrodes are formed by two pairs of comb electrodes interleaved with each other.
  • the first and second IDT electrodes are mutually connected. It may be formed by a pair of interdigital electrodes that are interleaved.
  • impedance matching with a circuit connected to the surface acoustic wave element tends to be difficult compared with the case where two pairs of comb-tooth electrodes are formed, but the submerged substance detection device 4 is realized with a simpler configuration. Therefore, it is easier to reduce the size of the apparatus.
  • the electrodes such as the first and second IDT electrodes 12 and 15 are made of, for example, an appropriate conductive material such as a metal such as Ag, Au, Pd, Pt, Al, Cu, or Ti, or an alloy such as Ag—Pd. Can be formed.
  • the electrodes such as the first and second IDT electrodes 12 and 15 may be formed of a conductive layer stack in which a plurality of conductive layers are stacked.
  • a protective film 20 is formed on the piezoelectric substrate 10.
  • the protective film 20 covers the first and second IDT electrodes 12 and 15 and the grating reflectors 13, 14, 16 and 17.
  • the protective film 20 is a layer for protecting the first and second IDT electrodes 12 and 15 and the grating reflectors 13, 14, 16, and 17 from liquids, dust, and the like.
  • the protective film 20 can be formed of an insulating material such as silicon oxide such as SiO 2 or silicon nitride such as SiN.
  • reaction film is a film that reacts with a substance in a liquid.
  • adsorption film is a film that adsorbs a substance in the liquid.
  • a substrate 30 is disposed on the surface acoustic wave element 10. This substrate 30 is for forming a detection recess for storing the liquid to be detected on the upper portions of the sensing units 18 and 19.
  • the substrate 30 has first and second openings 30a and 30b. These openings 30 a and 30 b are formed larger than the sensing portions 18 and 19.
  • the surface acoustic wave element 10 is mounted on the substrate 30 such that the openings 30 a and 30 b of the substrate 30 face the sensing units 18 and 19.
  • the substrate 30 is not particularly limited as long as the substrate 30 has rigidity capable of supporting the surface acoustic wave element 10.
  • the substrate 30 may be a substrate made of an inorganic material, a substrate made of an organic material, or a substrate containing both an inorganic material and an organic material.
  • the substrate 30 can be composed of, for example, a glass epoxy substrate, a glass substrate, a ceramic substrate, a resin substrate, or the like.
  • substrate 30 may be comprised with the film.
  • a conductive layer 31 is formed on the substrate 30.
  • the conductive layer 31 includes not only the surface 30c of the substrate 30 on the surface acoustic wave element 10 side, but also the inner surfaces of the first and second openings 30a and 30b, and the back surface of the substrate 30 opposite to the surface acoustic wave element 10 side. 30d is covered. Thereby, the deterioration by the corrosion of the board
  • substrate 30 is suppressed.
  • the conductive layer 31 includes a layer having excellent corrosion resistance such as an Au layer, deterioration of the substrate 30 due to corrosion can be more effectively suppressed.
  • deterioration due to corrosion of the substrate 30 is particularly likely to proceed on the inner surfaces of the first and second openings 30a and 30b that are in contact with the liquid, and therefore, the back surface 30d of the substrate 30 and the first and second openings 30a and 30b are not affected. It is preferable to form the conductive layer 31 on the inner surfaces, particularly on the inner surfaces of the first and second openings 30a and 30b.
  • the resin layer 40 is disposed between the substrate 30 and the surface acoustic wave element 10.
  • the substrate 30 and the surface acoustic wave element 10 are bonded by the resin layer 40.
  • the resin layer 40 is connected to the surface 30 c of the substrate 30 and the surface of the surface acoustic wave element 10. That is, the resin layer 40 is formed so as to reach the surface acoustic wave element 10 from the substrate 30.
  • the resin layer 40 is formed outside the sensing units 18 and 19. Specifically, the resin layer 40 is formed in an annular shape so as to surround the sensing units 18 and 19.
  • the resin layer 40 and the first and second openings 30 a and 30 b formed in the substrate 30 form first and second detection recesses 32 and 33.
  • the resin layer 40 is provided at a position retracted from the end surfaces of the openings 30a and 30b. That is, the resin layer 40 is formed so as not to be positioned in the openings 30a and 30b when viewed from the opening direction x of the openings 30a and 30b of the substrate 30. For this reason, the resin layer 40 is not formed on the periphery of the openings 30a and 30b of the surface 30c of the substrate 30.
  • the resin layer 40 is particularly limited as long as it can adhere the substrate 30 and the surface acoustic wave element 10 and has a certain degree of durability against the liquid supplied to the detection recesses 32 and 33.
  • the resin layer 40 may be, for example, a thermoplastic resin or an energy ray curable resin that is cured by energy rays.
  • the energy rays include heat rays and light rays.
  • the energy ray curable resin includes a thermosetting resin, a photocurable resin, and the like.
  • the resin layer 40 can be formed of, for example, an epoxy resin or a polyimide resin.
  • the wall surfaces of the detection recesses 32 and 33 are hydrophilic. Specifically, the surface of the conductive layer 31 constituting the wall surfaces of the detection recesses 32 and 33 has hydrophilicity.
  • a hydrophobic layer 45 having hydrophobicity is formed on at least one of the portions positioned on the detection recesses 32 and 33 side. Specifically, in the present embodiment, the hydrophobic layer 45 is formed on a portion of the surface 30c of the substrate 30 on the surface acoustic wave element 10 side that is located on the detection recesses 32 and 33 side of the resin layer 40. Has been.
  • the hydrophobic layer 45 is formed on a portion extending from the openings 30a and 30b of the surface 30c to the outside of the resin layer 40.
  • the portion of the hydrophobic layer 45 located inside the resin layer 40 is formed in an annular shape so as to surround the detection recesses 32 and 33.
  • the hydrophobic layer 45 can be formed of, for example, perfluoroalkylethyl acrylate or a fluorine-based resin containing a perfluoro group.
  • the hydrophobic layer 45 is provided. Therefore, the liquid to be detected injected into the detection recesses 32 and 33 is repelled by the hydrophobic layer 45. Therefore, the water-based detection liquid is effectively suppressed from reaching the resin layer 40 by the water repellent force of the hydrophobic layer 45. Accordingly, it is possible to effectively suppress the bleed material from the resin layer 40 from being mixed into the liquid to be detected located in the sensing units 18 and 19. As a result, the substance contained in the liquid to be detected can be detected with high detection accuracy.
  • the gap between the substrate 30 and the surface acoustic wave element 10 is determined by the water repellency of the hydrophobic layer 45 and the surface of the liquid to be detected. It is preferable that the distance is such that the liquid to be detected can be effectively prevented from entering the gap between the substrate 30 and the surface acoustic wave element 10 due to the tension.
  • the gap between the substrate 30 and the surface acoustic wave element 10 is preferably 100 ⁇ m or less.
  • the hydrophobic layer 45 is formed in an annular shape so as to surround the detection recesses 32 and 33. For this reason, it can suppress more reliably that a to-be-detected liquid reaches the resin layer 40.
  • the hydrophobic layer 45 is formed on the surface of the substrate 30 and is not formed on the surface of the surface acoustic wave element 10. For this reason, the characteristic change of the surface acoustic wave element 10 due to the formation of the hydrophobic layer 45 on the surface acoustic wave element 10 can be suppressed.
  • the hydrophobic layer 45 is not formed on the terminal portion 30c1 of the surface 30c of the substrate 30 to be electrically connected. For this reason, by providing the hydrophobic layer 45, electrical connection can be reliably performed.
  • the surfaces of the detection recesses 32 and 33 are hydrophilic, the liquid to be detected can be taken out and replaced stably.
  • FIG. 17 is a schematic cross-sectional view of the in-liquid substance detection device of the fifth embodiment.
  • the submerged substance detection device 5 according to the present embodiment is different from the submerged substance detection device 4 of the fourth embodiment in that a wall 46 is provided.
  • the wall portion 46 is formed so as to reach the surface acoustic wave element 10 from the substrate 30 in a portion located on the detection recesses 32 and 33 side with respect to the resin layer 40. For this reason, the resin layer 40 is isolated from the detection recesses 32 and 33 by the wall 46. Therefore, it can suppress more effectively that the bleed thing from the resin layer 40 mixes in a to-be-detected liquid.
  • the wall portion 46 can be formed of a material other than a resin that generates a bleed material, such as polyimide.
  • FIG. 18 is a schematic cross-sectional view of the in-liquid substance detection device of the sixth embodiment.
  • the hydrophobic layer 45 is formed only on the substrate 30 side.
  • the hydrophobic layer may be formed on both the substrate side and the surface acoustic wave element side.
  • the hydrophobic layer 45a is formed on the portion of the surface 30c of the substrate 30 on the surface acoustic wave element 10 side that is positioned on the detection recesses 32 and 33 side of the resin layer 40.
  • a hydrophobic layer 45b is formed on a portion of the surface acoustic wave element 10 located on the detection recesses 32 and 33 side of the surface of the substrate 30 side of the surface acoustic wave element 10.
  • the hydrophobic layer 45a and the hydrophobic layer 45b are opposed to each other.
  • the hydrophobic layer 45a on the substrate 30 side and the hydrophobic layer 45b on the surface acoustic wave element 10 side it is more effectively suppressed that the liquid to be detected reaches the resin layer 40. can do. Therefore, higher detection accuracy can be realized.
  • FIG. 19 is a schematic plan view of the in-liquid substance detection device according to the seventh embodiment.
  • FIG. 20 is a schematic plan view of the in-liquid substance detection device of the eighth embodiment.
  • FIG. 21 is a schematic plan view of the in-liquid substance detection device of the ninth embodiment.
  • the arrangement of the resin layer 40 and the hydrophobic layer 45 is not particularly limited as long as the hydrophobic layer 45 is located between the resin layer 40 and the detection recesses 32 and 33.
  • the resin layer 40 and the hydrophobic layer 45 may be arranged as shown in the seventh to ninth embodiments shown in FIGS.
  • the resin layer 40 and the hydrophobic layer 45 are formed concentrically. In this way, by forming the resin layer 40 in an annular shape, when the liquid to be detected is put, the space between the liquid to be detected, the resin layer 40, the substrate 30, and the surface acoustic wave element 10 and only air exists. By being formed, it is possible to effectively suppress wetting and spreading on the substrate 30 or the surface of the surface acoustic wave element 10.
  • the resin layer 40 is not formed so as to surround the detection recesses 32 and 33.
  • the resin layer 40 is formed in a rectangular shape.
  • Example 10 Ten actual submerged substance detection devices 3 shown in FIG. 11 are produced by the manufacturing method described in the second embodiment, and water is put into the detection recesses 32 and 33 for each sample. The substance was detected. Specifically, the transmission frequencies of the sensing units 18 and 19 were measured, and the amount of frequency change from the transmission frequency at the start of measurement was monitored over time. The result is shown in FIG. In the present embodiment, an epoxy underfill is used as the resin layer 40. The hydrophobizing treatment was performed with non-bleed N-11. The hydrophilic treatment was performed by UV / ozone irradiation.
  • the frequency change amount increased with time. Moreover, the frequency change amount of the transmission frequency greatly differs depending on the sample. This result shows that the substance in the liquid cannot be detected stably.
  • Substance detection apparatus 10 Surface acoustic wave element 11 ... Piezoelectric substrate 12 ... 1st IDT electrode 12a, 12b, 12c, 12d ... Comb electrode 12e ... 1st input / output port 12f, 12h ... Ground Port 12g ... second input / output port 13,14 ... grating reflector 15 ... second IDT electrodes 15a, 15b, 15c, 15d ... comb electrode 15e, 15g ... ground port 15g ... first input / output port 15h ... Second input / output ports 16, 17 ... grating reflectors 18, 19 ... sensing unit 20 ...

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  • Physics & Mathematics (AREA)
  • Acoustics & Sound (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Materials By The Use Of Ultrasonic Waves (AREA)

Abstract

La présente invention concerne un dispositif permettant de détecter une substance dans un liquide, capable d'assurer une détection stable et précise d'une substance. L'invention concerne également un procédé de fabrication de ce dispositif. Ledit dispositif (1) comprend : un substrat (30) dans lequel sont formées des ouvertures (30a, 30b) ; un élément à onde de surface élastique (10) qui possède un substrat piézoélectrique (11), possède des électrodes IDT (12, 15) qui constituent des parties de détection (18, 19) et qui est monté sur le substrat (30) de sorte que les parties de détection (18, 19) soient face aux ouvertures (30a, 3b) dans le substrat (30) ; et une couche de résine (40) formée entre le substrat (30) et l'élément à onde de surface élastique (10) de manière à entourer les parties de détection (18, 19). Le dispositif de l'invention permettant de détecter une substance dans un liquide est fabriqué par : la préparation d'une structure montée (42) dans laquelle l'élément à onde de surface élastique (10) est monté sur le substrat (30), dont au moins les surfaces intérieures des ouvertures (30a, 30b) sont hydrophobes ; la formation de la couche de résine (40) dans la structure montée (42) ; et l'hydrophilisation des surfaces des dépressions de détection (32, 33).
PCT/JP2010/067626 2009-10-13 2010-10-07 Dispositif permettant de détecter une substance dans un liquide et procédé de fabrication associé WO2011046059A1 (fr)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013152209A (ja) * 2011-12-27 2013-08-08 Kyocera Corp 弾性表面波センサおよびその製造方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH11153582A (ja) * 1997-11-21 1999-06-08 Japan Science & Technology Corp 液体物性の測定方法とその装置
WO2006018981A1 (fr) * 2004-08-05 2006-02-23 Sony Corporation Procédé de fabrication d’une puce à adn, système de fabrication, procédé de détection d’hybridation, système de détection, dispositif de traitement de substrat, et procédé de traitement de substrat
JP3952083B2 (ja) * 2004-09-10 2007-08-01 株式会社村田製作所 液中物質検出センサ及びそれを用いた液中物質検出装置

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH11153582A (ja) * 1997-11-21 1999-06-08 Japan Science & Technology Corp 液体物性の測定方法とその装置
WO2006018981A1 (fr) * 2004-08-05 2006-02-23 Sony Corporation Procédé de fabrication d’une puce à adn, système de fabrication, procédé de détection d’hybridation, système de détection, dispositif de traitement de substrat, et procédé de traitement de substrat
JP3952083B2 (ja) * 2004-09-10 2007-08-01 株式会社村田製作所 液中物質検出センサ及びそれを用いた液中物質検出装置

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013152209A (ja) * 2011-12-27 2013-08-08 Kyocera Corp 弾性表面波センサおよびその製造方法

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