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WO2025142975A1 - Dispositif, et appareil de mesure de concentration le comprenant, et procédé de mesure de concentration l'utilisant - Google Patents

Dispositif, et appareil de mesure de concentration le comprenant, et procédé de mesure de concentration l'utilisant Download PDF

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Publication number
WO2025142975A1
WO2025142975A1 PCT/JP2024/045805 JP2024045805W WO2025142975A1 WO 2025142975 A1 WO2025142975 A1 WO 2025142975A1 JP 2024045805 W JP2024045805 W JP 2024045805W WO 2025142975 A1 WO2025142975 A1 WO 2025142975A1
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WIPO (PCT)
Prior art keywords
gate electrode
concentration
threshold voltage
electrodes
pair
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PCT/JP2024/045805
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English (en)
Japanese (ja)
Inventor
成紀 徳地
篤郎 住吉
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Mitsui Kinzoku Co Ltd
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Mitsui Mining and Smelting Co Ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/403—Cells and electrode assemblies
    • G01N27/414—Ion-sensitive or chemical field-effect transistors, i.e. ISFETS or CHEMFETS

Definitions

  • a gate electrode 102 is formed on a substrate 101, and an insulating film 103 is formed so as to cover this gate electrode 102.
  • a semiconductor layer 104 is formed on the insulating film 103, and a drain electrode 105 and a source electrode 106 are formed so as to be in contact with the semiconductor layer 104.
  • Patent Documents 1 and 2 an oxide semiconductor containing indium (In) and zinc (Zn) and also containing gallium (Ga), aluminum (Al), iron (Fe), etc., particularly an oxide semiconductor containing In, Ga, and Zn (hereinafter referred to as "InGaZnO"), is used as the semiconductor layer 104.
  • crystalline Si silicon has often been used as the semiconductor layer 104.
  • InGaZnO is transparent to visible light and flexible, so its applications are not limited.
  • its OFF current is approximately 1.0 ⁇ 10 ⁇ 16 A/ ⁇ m to 1.0 ⁇ 10 ⁇ 11 A/ ⁇ m, which is smaller than that of crystalline Si, so that the effect of noise during measurement is small.
  • InGaZnO has a low field effect mobility of approximately 10 cm 2 /Vs, it is difficult to accurately detect changes in the threshold voltage V th unless the drain-source voltage V DS is made sufficiently large.
  • a device comprising an insulating substrate, a gate electrode formed on the insulating substrate, at least one insulating composite layer formed on the gate electrode in a state insulated from the gate electrode, and a reservoir capable of holding a test fluid
  • the insulating composite layer has a pair of electrodes and a semiconductor layer in contact with the pair of electrodes, the semiconductor layer being composed of an oxide containing indium (In), zinc (Zn) and an additive element (X);
  • the additive element (X) includes at least one element selected from tantalum (Ta), strontium (Sr), and niobium (Nb),
  • a device comprising a sensitive membrane between the insulating composite layer and the reservoir, the sensitive membrane being selective for a target substance in the test fluid.
  • a device includes: a voltage application means for varying a voltage applied between the electrode into which a current flows out of the pair of electrodes and the gate electrode; a current measuring means for measuring a current flowing between the pair of electrodes; a threshold voltage detection means for detecting a threshold voltage Vth, which is a voltage value of the gate electrode when a current flows between the pair of electrodes, based on a voltage value applied by the voltage application means and a current value measured by the current measurement means; and a concentration calculation means for calculating the concentration of the target substance in the test fluid based on the threshold voltage Vth detected by the threshold voltage detection means.
  • FIG. 1 is a schematic diagram for explaining the configuration of a concentration measuring device according to the present embodiment.
  • FIG. 2 is a schematic front view for explaining the configuration of a device used in the concentration measuring apparatus of FIG.
  • FIG. 3 is a schematic side view of FIG.
  • FIG. 4 is a graph showing the relationship between the concentration of the target substance in the sample liquid L and the threshold voltage Vth when the concentration of the target substance in the sample liquid L is measured using the concentration measuring device of FIG.
  • FIG. 5 is a schematic diagram for explaining the configuration of a conventional sensor having a FET structure.
  • FIG. 1 is a schematic diagram for explaining the configuration of a concentration measuring apparatus in this embodiment
  • FIG. 2 is a schematic front view for explaining the configuration of a device used in the concentration measuring apparatus of FIG. 1
  • FIG. 3 is a schematic side view of FIG. 2.
  • the gate electrode layer 13 has a gate electrode 131 formed on the insulating substrate 12, and an insulating film 132.
  • an insulating film 12a is provided between the insulating substrate 12 and the gate electrode 131 to prevent the intrusion of various gases, water vapor, and the like, but the gate electrode 131 can also be formed directly on the insulating substrate 12.
  • the liquid storage section 16 is not particularly limited as long as it is configured to hold the sample liquid L, but in this embodiment, it is configured with a partition section 16a that is provided to surround the sensitive membrane 18 in order to hold the sample liquid L so that the sample liquid L comes into contact with the sensitive membrane 18 described below.
  • the concentration of the target substance contained in the target substance contained in the target substance liquid L is measured by storing the target substance liquid L in the storage section 16 as the test fluid.
  • a storage section capable of storing gas instead of the storage section 16, and store the target substance liquid L in the storage section as the test fluid, thereby measuring the concentration of the target substance contained in the gas.
  • a sensitive membrane 18 is provided between the insulating composite layer 14 and the liquid storage portion 16 .
  • the sensitive membrane 18 has selectivity for the target substance in the sample liquid L. Specifically, it has the property of selectively transmitting ions of the target substance and selectively capturing components of the target substance (e.g., nucleic acid).
  • a sensitive membrane 18 for example, ionophores such as lithium ionophore, potassium ionophore, sodium ionophore, calcium ionophore, ammonium ionophore, ionophore for chloride ions, magnesium ionophore, etc. can be used, or a lipid membrane or a nucleic acid probe can be used.
  • the method for producing such a sensitive film 18 is not particularly limited, but for example, when an ionophore is used, the sensitive film 18 can be produced by the following steps. First, polyvinyl chloride is weighed out into a beaker. In this case, it is preferable to use polyvinyl chloride with a degree of polymerization of about 1050 from the viewpoints of ease of handling and smooth application to the insulating composite layer 14.
  • plasticizer for example, 2-nitrophenyl octyl ether (NPOE), bis(2-ethylhexyl) sebacate, or the like can be used.
  • NPOE 2-nitrophenyl octyl ether
  • anion scavenger for example, potassium tetrakis(4-chlorophenyl)borate can be used, and as a cation scavenger, for example, tridodecylmethylammonium chloride (TDDMACl) can be used.
  • TDDMACl tridodecylmethylammonium chloride
  • the ionophore can be appropriately selected depending on the ion to be detected.
  • dibenzyl-14-crown-4 or TTD-14-crown-4 can be used to detect lithium ions (Li + )
  • bis(benzo-15 - crown-5) can be used to detect potassium ions (K + )
  • bis(12-crown-4) can be used to detect sodium ions (Na + )
  • HDOPP-Ca can be used to detect calcium ions (Ca 2+ )
  • nonactin can be used to detect ammonium ions (NH 4 + )
  • Bisthiourea-1 can be used to detect chloride ions (Cl - )
  • C14-K22B5, K22B1B5, or K22B9 can be used to detect magnesium ions (Mg 2+ ).
  • the solution thus prepared is spread on a glass petri dish and air-dried to create the sensitive film 18.
  • the response speed establishment of ion diffusion equilibrium
  • the insulating composite layer 14 is provided with an insulating film 146 at least at a portion in contact with the sensitive film 18.
  • the insulating film 146 also serves as a protective layer for protecting the semiconductor layer 144 from the sample liquid L. By providing the insulating film 146, the semiconductor layer 144 can be prevented from being corroded, and the durability and reliability of the semiconductor layer 144 can be improved. Any known material having insulating properties can be used as the material for the insulating film 146, and a material having corrosion resistance is preferable.
  • the semiconductor layer 144 preferably has a field effect mobility of 20 cm 2 /Vs or more, and more preferably 60 cm 2 /Vs or more.
  • Such a semiconductor layer 144 is composed of an oxide containing indium (In), zinc (Zn) and an additive element (X), where the additive element (X) is at least one element selected from tantalum (Ta), strontium (Sr) and niobium (Nb).
  • the atomic ratio of In and X satisfy the following formula (1) (X in the formula is the sum of the content ratios of the additive elements. The same applies to formulas (2) and (3) below). 0.4 ⁇ (In+X)/(In+Zn+X) ⁇ 0.8 (1) It is preferable that Zn satisfies the atomic ratio represented by the following formula (2). 0.2 ⁇ Zn/(In+Zn+X) ⁇ 0.6 (2) It is preferable that X satisfies the atomic ratio represented by the following formula (3). 0.001 ⁇ X/(In+Zn+X) ⁇ 0.015 (3)
  • the atomic ratio of In, Zn and X satisfy formula (1-3), formula (2-3) or formula (3-3). 0.48 ⁇ (In+X)/(In+Zn+X) ⁇ 0.78 (1-3) 0.22 ⁇ Zn/(In+Zn+X) ⁇ 0.52 (2-3) 0.002 ⁇ X/(In+Zn+X) ⁇ 0.012 (3-3)
  • the thinner the thickness of the semiconductor layer 144 the greater the change in the conductivity of the surface layer, and therefore the greater the change in the moving charge, as described below, and the improved measurement accuracy.
  • the thickness of such a semiconductor layer 144 is preferably 0.5 ⁇ m or less, more preferably 0.1 ⁇ m or less, and particularly preferably 0.05 ⁇ m or less. There is no particular lower limit for the thickness of the semiconductor layer 144, but it is generally 0.005 ⁇ m or more.
  • the device 10 described above is formed as a FET structure, it can be formed using a method similar to that used for conventionally known FETs and MOSFETs.
  • a conductive metal thin film is formed as the first electrode 141 and the second electrode 142 on the insulating substrate 12 using a sputtering device, and then an oxide thin film having the above-described configuration is formed as the semiconductor layer 144 using a sputtering device.
  • a shadow mask can be used for patterning in the formation of the first electrode 141 and the second electrode 142 and the formation of the semiconductor layer 144.
  • the conductive metal used as the first electrode 141 and the second electrode 142 is not particularly limited, but may be, for example, molybdenum (Mo) or tungsten (W), or an alloy of these metals with cerium oxide ( CeO2 ), copper (Cu), silver (Ag), or the like.
  • a ceramic thin film can be deposited thereon to form the insulating film 146.
  • a plasma CVD apparatus such as Samco Corporation's PD-2202L can be used to deposit a SiOx thin film under the conditions of a deposition gas: SiH4 / N2O / N2 mixed gas, a deposition pressure: 110 Pa, and a substrate temperature of 250°C to 400°C, to form the insulating film 146.
  • the control device 60 of the concentration measuring device 50 of this embodiment also includes a variable voltage source 32 for applying a voltage between the first electrode 141 and the second electrode 142, a variable voltage source 34 (voltage application means) for applying a voltage between the first electrode 141 and the gate electrode 131, an ammeter 36 (current measurement means) for measuring the current value between the first electrode 141 and the second electrode 142, and a voltmeter 38 (voltage measurement means) for measuring the voltage value between the first electrode 141 and the gate electrode 131.
  • a variable voltage source 32 for applying a voltage between the first electrode 141 and the second electrode 142
  • a variable voltage source 34 voltage application means
  • ammeter 36 current measurement means
  • a voltmeter 38 voltage measurement means
  • the control device 60 has a computer equipped with a calculation means, a storage means, an input/output means, etc., and is configured to control the applied voltage of the variable voltage source 32 and the variable voltage source 34, measure the current value with the ammeter 36, and measure the voltage value with the voltmeter 38 based on a program stored in the storage means.
  • the control device 60 further includes a threshold voltage detection means 62.
  • the threshold voltage detection means 62 is configured to control the voltages applied by the variable voltage sources 32 and 34, and to receive the current and voltage values measured by the ammeter 36 and voltmeter 38 as electrical signals.
  • Such a threshold voltage detection means 62 can be realized by a computer incorporated in the control device 60, etc.
  • the threshold voltage detection means 62 gradually increases the voltage Vg applied between the first electrode 141 and the gate electrode 131 by the variable voltage source 34 while a predetermined voltage Vds is applied between the first electrode 141 and the second electrode 142 by the variable voltage source 32. Then, the threshold voltage detection means 62 measures the threshold voltage Vth by detecting a change in the current Id flowing between the first electrode 141 and the second electrode 142 by the ammeter 36 and detecting a change in the voltage Vg between the first electrode 141 and the gate electrode 131 by the voltmeter 38.
  • the threshold voltage Vth varies depending on the amount of the analyte present on the surface of the sensitive membrane 18 or inside the sensitive membrane 18. Therefore, by measuring this threshold voltage Vth , the concentration of the analyte contained in the sample liquid L can be detected.
  • the method of measuring the threshold voltage Vth is not particularly limited, and may be, for example, detecting the voltage Vg when the current Id starts to flow between the first electrode 141 and the second electrode 142, or detecting the voltage Vg when the current Id stops flowing by gradually decreasing the voltage Vg from a state in which the current Id is flowing.
  • a predetermined value e.g. 1 ⁇ 10 ⁇ 9 A
  • FIG. 4 is a graph showing the relationship between the concentration of the target substance in the sample liquid L and the threshold voltage Vth when the concentration of the target substance in the sample liquid L is measured using the concentration measuring device 50 of this embodiment.
  • the sample liquid L was an aqueous solution of ammonium chloride ( NH4Cl )
  • the object to be detected was ammonium ion ( NH4 + )
  • the sensitive membrane 18 was an ammonium ionophore
  • the voltage Vds was 1 V
  • the voltage Vg was changed within a predetermined range of 1.3 V to 1.5 V.
  • the concentration of the analyte to be detected can be obtained based on the threshold voltage Vth measured using the concentration measuring device 50.
  • AI artificial intelligence
  • the control device 60 of this embodiment further includes a concentration calculation means 64, which is configured to calculate the concentration of the detection target as described above, based on the threshold voltage Vth detected by the threshold voltage detection means 62.
  • concentration calculation means 64 can be realized by a computer incorporated in the control device 60, etc.

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Abstract

Le problème à résoudre par la présente invention est de fournir un dispositif utilisable pour un appareil de mesure de concentration et un procédé de mesure de concentration qui permettent de détecter une tension de seuil Vth avec une sensibilité élevée et de mesurer rapidement la concentration de cible de détection dans un fluide échantillon même si la quantité de la cible de détection dans le fluide échantillon est minuscule. La solution selon l'invention porte sur un dispositif qui comprend : un substrat isolant ; une électrode de grille formée sur le substrat isolant ; au moins une couche composite isolante formée dans un état isolé sur l'électrode de grille ; et une partie de stockage apte à contenir un fluide échantillon. La couche composite isolante comporte une paire d'électrodes et une couche semi-conductrice en contact avec la paire d'électrodes. La couche semi-conductrice est composée d'un oxyde comprenant de l'indium élémentaire (In), du zinc élémentaire (Zn) et un élément additif (X). L'élément additif (X) comprend au moins un élément choisi parmi le tantale (Ta), le strontium (Sr) et le niobium (Nb). Le dispositif comprend, entre la couche composite isolante et la partie de stockage, un film sensible qui présente une sélectivité par rapport à une cible de détection dans le fluide échantillon.
PCT/JP2024/045805 2023-12-28 2024-12-25 Dispositif, et appareil de mesure de concentration le comprenant, et procédé de mesure de concentration l'utilisant Pending WO2025142975A1 (fr)

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Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012047763A (ja) * 2011-12-09 2012-03-08 Dainippon Printing Co Ltd 電界効果トランジスタ型バイオセンサ
JP2013092480A (ja) * 2011-10-26 2013-05-16 Dainippon Printing Co Ltd バイオセンサ測定装置及びその測定方法
KR20150005772A (ko) * 2013-07-04 2015-01-15 연세대학교 산학협력단 용액 공정 기반 적층형 산화물 박막 트랜지스터 바이오 센서 및 그를 제조하는 제조 방법
WO2018025647A1 (fr) * 2016-08-03 2018-02-08 株式会社ニコン Dispositif à semi-conducteur, capteur de ph, biocapteur, et procédé de production de dispositif à semi-conducteur
US20180095052A1 (en) * 2016-09-30 2018-04-05 Seung Ik Jun Biosensor
JP2020513684A (ja) * 2016-11-14 2020-05-14 アルマ マータ ストゥディオルム−ウニベルシータ ディ ボローニャＡｌｍａ Ｍａｔｅｒ Ｓｔｕｄｉｏｒｕｍ − Ｕｎｉｖｅｒｓｉｔａ’ Ｄｉ Ｂｏｌｏｇｎａ 感応性電界効果デバイス及びその製造方法
JP2021105564A (ja) * 2019-12-26 2021-07-26 Ｔｉａｎｍａ Ｊａｐａｎ株式会社 イオンセンサ装置
JP7364824B1 (ja) * 2022-01-31 2023-10-18 三井金属鉱業株式会社 電界効果トランジスタ及びその製造方法並びに電界効果トランジスタ製造用スパッタリングターゲット材
WO2024024637A1 (fr) * 2022-07-29 2024-02-01 三井金属鉱業株式会社 Dispositif, appareil de mesure de concentration d'ions hydroxyde le comprenant, et procédé de mesure de concentration d'ions hydroxyde à l'aide dudit dispositif

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013092480A (ja) * 2011-10-26 2013-05-16 Dainippon Printing Co Ltd バイオセンサ測定装置及びその測定方法
JP2012047763A (ja) * 2011-12-09 2012-03-08 Dainippon Printing Co Ltd 電界効果トランジスタ型バイオセンサ
KR20150005772A (ko) * 2013-07-04 2015-01-15 연세대학교 산학협력단 용액 공정 기반 적층형 산화물 박막 트랜지스터 바이오 센서 및 그를 제조하는 제조 방법
WO2018025647A1 (fr) * 2016-08-03 2018-02-08 株式会社ニコン Dispositif à semi-conducteur, capteur de ph, biocapteur, et procédé de production de dispositif à semi-conducteur
US20180095052A1 (en) * 2016-09-30 2018-04-05 Seung Ik Jun Biosensor
JP2020513684A (ja) * 2016-11-14 2020-05-14 アルマ マータ ストゥディオルム−ウニベルシータ ディ ボローニャＡｌｍａ Ｍａｔｅｒ Ｓｔｕｄｉｏｒｕｍ − Ｕｎｉｖｅｒｓｉｔａ’ Ｄｉ Ｂｏｌｏｇｎａ 感応性電界効果デバイス及びその製造方法
JP2021105564A (ja) * 2019-12-26 2021-07-26 Ｔｉａｎｍａ Ｊａｐａｎ株式会社 イオンセンサ装置
JP7364824B1 (ja) * 2022-01-31 2023-10-18 三井金属鉱業株式会社 電界効果トランジスタ及びその製造方法並びに電界効果トランジスタ製造用スパッタリングターゲット材
WO2024024637A1 (fr) * 2022-07-29 2024-02-01 三井金属鉱業株式会社 Dispositif, appareil de mesure de concentration d'ions hydroxyde le comprenant, et procédé de mesure de concentration d'ions hydroxyde à l'aide dudit dispositif

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
徳地成紀 他, セラミックス産業を科学技術で支える企業たち, 三井金属鉱業株式会社－高移動度酸化物半導体の開発－, セラミックス, 01 March 2023, vol. 58, no. 3, pp. 136-138, (TOKUCHI, Shigeki et al., Mitsui Mining & Smelting Co., LTD.-The Development of High-Mobility Oxide Semiconductor-, Bulletin of the Ceramic Society of Japan) *

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