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WO2007105141A2 - Capteur magnétique à stabilisation de gain - Google Patents

Capteur magnétique à stabilisation de gain Download PDF

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Publication number
WO2007105141A2
WO2007105141A2 PCT/IB2007/050711 IB2007050711W WO2007105141A2 WO 2007105141 A2 WO2007105141 A2 WO 2007105141A2 IB 2007050711 W IB2007050711 W IB 2007050711W WO 2007105141 A2 WO2007105141 A2 WO 2007105141A2
Authority
WO
WIPO (PCT)
Prior art keywords
sensor
magnetic
magnetic sensor
noise
gain
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/IB2007/050711
Other languages
English (en)
Other versions
WO2007105141A3 (fr
Inventor
Josephus Arnoldus Henricus Maria Kahlman
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Koninklijke Philips NV
Original Assignee
Koninklijke Philips Electronics NV
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Koninklijke Philips Electronics NV filed Critical Koninklijke Philips Electronics NV
Publication of WO2007105141A2 publication Critical patent/WO2007105141A2/fr
Publication of WO2007105141A3 publication Critical patent/WO2007105141A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R33/00—Arrangements or instruments for measuring magnetic variables
    • G01R33/02—Measuring direction or magnitude of magnetic fields or magnetic flux
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/06—Investigating concentration of particle suspensions
    • G01N15/0656—Investigating concentration of particle suspensions using electric, e.g. electrostatic methods or magnetic methods
    • 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
    • G01N27/72—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating magnetic variables
    • G01N27/74—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating magnetic variables of fluids
    • G01N27/745—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating magnetic variables of fluids for detecting magnetic beads used in biochemical assays
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/48—Biological material, e.g. blood, urine; Haemocytometers
    • G01N33/50—Chemical analysis of biological material, e.g. blood, urine; Testing involving biospecific ligand binding methods; Immunological testing
    • G01N33/53—Immunoassay; Biospecific binding assay; Materials therefor
    • G01N33/543—Immunoassay; Biospecific binding assay; Materials therefor with an insoluble carrier for immobilising immunochemicals
    • G01N33/54313—Immunoassay; Biospecific binding assay; Materials therefor with an insoluble carrier for immobilising immunochemicals the carrier being characterised by its particulate form
    • G01N33/54326—Magnetic particles
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R33/00—Arrangements or instruments for measuring magnetic variables
    • G01R33/02—Measuring direction or magnitude of magnetic fields or magnetic flux
    • G01R33/06—Measuring direction or magnitude of magnetic fields or magnetic flux using galvano-magnetic devices
    • G01R33/09—Magnetoresistive devices
    • 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
    • G01N35/0098—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor involving analyte bound to insoluble magnetic carrier, e.g. using magnetic separation

Definitions

  • the invention relates to a magnetic sensor device comprising at least one magnetic sensor element for providing a sensor signal. Moreover, the invention relates to the use of such a magnetic sensor device and a method for measuring magnetic fields with such a magnetic sensor device.
  • a magnetic sensor device which may for example be used in a microfluidic biosensor for the detection of (e.g. biological) molecules labeled with magnetic beads.
  • the microsensor device is provided with an array of sensor units comprising wires for the generation of a magnetic field and Giant Magneto Resistance devices (GMRs) for the detection of stray fields generated by magnetized beads. The resistance of the GMRs is then indicative of the number of the beads near the sensor unit.
  • GMRs Giant Magneto Resistance devices
  • a problem with magnetic biosensors of the aforementioned kind is that the sensitivity of the magneto -resistive elements and therefore the effective gain of the whole measurements is very sensitive to uncontrollable parameters like magnetic instabilities in the sensors, external magnetic fields, aging, temperature and the like.
  • the magnetic sensor device comprises the following components: a) At least one magnetic sensor element for providing a sensor signal, wherein said sensor signal is indicative of a magnetic field (or at least a
  • the magnetic sensor element is (at least partially) exposed to.
  • An evaluation unit that is coupled to the magnetic sensor element and that is adapted to measure the amount of noise in a given spectral range of the sensor signal.
  • amount of noise refers to a measure that has to be predefined.
  • the amount of noise may for example be
  • the magnetic sensor element can be driven by a sensor current, and the noise is an 1/f noise that is associated with the sensor current. If the magnetic sensor element is for example a magneto -resistive element and the sensor
  • the 1/f noise is the result of the noise resistance spectral density (nRSD) of this element.
  • This noise has a magnetic origin and a 1/f character, multiplied by the sensor current I 2 which is applied to the magneto -resistive element. If the sensor current is modulated by some frequency f 2 , the 1/f resistance noise R nO ise is shifted in the spectrum of the sensor voltage U nO ise according to the relation
  • the (l/f) noise is often suppressed and/or measurements are deliberately made in a spectral range where the (1/f) noise can be neglected.
  • the magnetic sensor device described above explicitly determines the amount of (1/f) noise because it turns out that this quantity comprises
  • the magnetic sensor element may be realized by a magneto -resistive element.
  • This may for example be a Giant Magnetic Resistance (GMR) element, a TMR (Tunnel Magneto Resistance) element, or an AMR (Anisotropic
  • the evaluation unit may optionally comprise a filter for selecting a frequency range around the centre of the observed noise.
  • the evaluation unit is adapted to calculate a value that represents the amount of noise in the sensor signal as the root- mean-square (RMS) value of the sensor signal in a given spectral interval around the centre of the noise.
  • said value may be defined as the peak value of the sensor signal in the aforementioned interval.
  • RMS root- mean-square
  • the evaluation unit is preferably adapted to calculate also the sensor gain of the magnetic sensor element. This calculation may particularly be based on the determined amount of noise, as this directly depends on the sensor gain.
  • the sensor gain is as usual defined as the derivative of the sensor signal (e.g. a voltage) with respect to the quantity to be measured (e.g. a magnetic field strength). The sensor gain therefore comprises every process between the quantity to be measured and the sensor signal.
  • the magnetic sensor device comprises a normalizing unit which is coupled to the evaluation unit and which can calibrate the (whole) sensor signal according to the calculated sensor gain.
  • the measurements that are encoded in the sensor signals
  • the magnetic sensor device comprises a normalizing unit which is coupled to the evaluation unit and which can calibrate the (whole) sensor signal according to the calculated sensor gain.
  • the magnetic sensor device comprises at least one magnetic field generator, for example a conductor wire, for generating a magnetic field in the surroundings of the magnetic sensor element.
  • the magnetic field generator can for example provoke magnetic reactions of a sample which are then detected by the magnetic sensor element. It may integrated into one chip with the sensor element, or it may be an external component of the sensor device.
  • the invention further relates to a method for measuring magnetic fields with at least one magnetic sensor element, particularly a magnetic sensor element of the kind described above.
  • the method comprises the measurement of the amount of noise in the sensor signal of the magnetic sensor element in a given spectral range.
  • the magnetic sensor element is provided with a sensor current, and the noise is a 1/f noise that is associated with the sensor current.
  • the method comprises in general form the steps that can be executed with a magnetic sensor device of the kind described above. Therefore, reference is made to the preceding description for more information on the details, advantages and improvements of that method.
  • the sensor gain is calculated from the measured amount of noise.
  • the sensor noise is exploited to extract useful information about the sensor characteristics.
  • the calculated sensor gain is preferably used to normalize sensor measurements and thus to make them independent of gain variations.
  • the invention further relates to the use of the magnetic sensor device described above for molecular diagnostics, biological sample analysis, or chemical sample analysis.
  • Molecular diagnostics may for example be accomplished with the help of magnetic beads that are directly or indirectly attached to target molecules.
  • Figure 1 depicts a block diagram of a magnetic sensor device according to the present invention
  • Figure 2 depicts the resistance of a GMR sensor as a function of the magnetic field in the sensitive layer of the GMR stack.
  • FIG. 1 illustrates a microelectronic magnetic sensor device according to the present invention in the particular application as a biosensor for the detection of magnetically interactive particles, e.g. superparamagnetic beads 2, in a sample chamber.
  • Magneto -resistive biochips or biosensors have promising properties for bio-molecular diagnostics, in terms of sensitivity, specificity, integration, ease of use, and costs. Examples of such biochips are described in the WO 2003/054566, WO 2003/054523, WO 2005/010542 A2, WO 2005/010543 Al, and WO 2005/038911 Al, which are incorporated into the present application by reference.
  • the magnetic sensor device 10 shown in Figure 1 comprises at least one magnetic field generator which may be realized as a conductor wire 11 on a substrate (not shown) or which may be located outside the sensor chip.
  • the generated external magnetic field H ext magnetizes magnetic beads 2 in the sample chamber, wherein said beads 2 may for instance be used as labels for (bio- )molecules of interest (for more details see cited literature). Magnetic stray fields generated by the beads 2 then affect (together with the excitation field H ext ) the electrical resistance of the nearby Giant Magneto Resistance (GMR) sensor element 12.
  • GMR Giant Magneto Resistance
  • an alternating or direct current I 2 I 2 o-sin(2 ⁇ f 2 t) of frequency f 2 is conducted through the GMR sensor element 12 by a further current source 22.
  • the voltage drop U GMR across the GMR sensor 12 is then a suitable sensor signal indicative of the resistance of the GMR sensor 12 and thus of the magnetic fields it is subjected to.
  • Figure 2 shows in this context the GMR resistance R as a function of the magnetic field H in the sensitive layer of the GMR stack.
  • the slope of the curve corresponds to the sensitivity S GMR of the magnetic sensor element 12.
  • the sensitivity S GMR and therefore the effective gain (i.e. the derivative du G MR/dH) of the measurement is sensitive to non-controllable parameters, for example: non-stochastic sensitivity variations due to magnetic instabilities in the sensor (this error cannot be removed by using a reference sensor or a bridged structure); - externally applied magnetic fields; production tolerances; aging effects; temperature; memory effects from e.g. magnetic actuation fields; gain variations in the current sources.
  • internal compensation techniques for magnetic and capacitive crosstalk will fail when the GMR sensitivity varies. It is therefore desirable to stabilize the sensor gain during an actual measurement, which can be achieved by measuring it.
  • the aforementioned aim and an unambiguous measure for the sensor gain can be achieved by continuously measuring the amount of low- frequency (1/f) noise.
  • This approach is based on the recognition that low- frequency 1/f noise is caused by random rotations of the magnetic domains in the free layer of the GMR sensor 12 which introduce an internal magnetic field H mt in the sensitive layer of said sensor.
  • the 1/f content in the read-out sensor signal U GMR is a direct measure for the gain of the GMR.
  • This idea fits well in the architecture of the magnetic biosensor where the 1/f regime is avoided for detection in order to achieve the highest possible detection signal- to-noise ratio.
  • the circuitry on the right-hand side of Figure 1 shows a particular embodiment of the aforementioned concepts.
  • the circuitry comprises a lower branch with an evaluation unit 30 which receives the sensor signal (voltage) U GMR as input and which comprises the following components: a band-pass filter 31 with a bandwidth typically ranging from ⁇ 0.01 kHz to ⁇ 0.1 MHz. a (low-noise) amplifier 32; - a processing circuit 33.
  • the band-pass filter 31 has a passband from e.g. 0.01 to 100 kHz which passes the desired 1/f noise spectrum and obviously blocks the large DC component. Moreover, the band-pass filter 31 should block the frequency f ⁇ (which contains the magnetic signal and parasitic crosstalk) and the thermal noise above the turnover point where the 1/f noise is no longer dominant. The bandpass filter thus limits the sensor spectrum to the 1/f frequency band of interest.
  • the modulation of the sensor current with a frequency f 2 > 0 is used to distinguish between the large parasitic (capacitive and inductive) crosstalk at fi and the desired signal at f i ⁇ f 2 in the detection chain, which allows to remove the crosstalk component by filtering in the frequency domain.
  • the 1/f spectrum shifts to sidebands around f 2 , wherein the spectral content of these sidebands comprises the desired gain information.
  • the sidebands can be isolated with an appropriate choice of the band-pass filter 31, the removal of f 2 (i.e. the center of the sidebands) may be implemented by adding a demodulation step at f 2 in the evaluation unit 30, e.g. before the BPF 31 (not shown).
  • Figure 1 is only indicative. Thus it is particularly possible to combine components from the detection chain (23 .. 27) and the gain measurement chain (31 .. 33).
  • the GMR resistance R fluctuates accordingly and proportional to its sensitivity S GMR .
  • the 1/f noise content detection criterion may for instance be the RMS signal value or the peak value in a certain bandwidth.
  • the excitation field H ext may be switched on or off during such a gain measurement. From the amount of 1/f noise, the sensor gain can readily be determined (e.g. by multiplying it with an appropriate constant). It should be noted that the sensor gain comprises everything between the internal 1/f magnetic field and the sensor voltage U GMR . Thus for example also variations of the current source 22 are captured by the proposed approach and stabilized.
  • the upper branch (detection chain) of the circuitry shown in Figure 1 comprises the usual components for processing the sensor voltage U GMR , namely: a (high-pass) filter 23; an amplifier 24; - a demodulator 25 for extracting the measurement signal of interest from the spectrum of the sensor signal U GMR ; a (low-pass) filter 26.
  • a normalizing unit 27 in the upper branch receives the sensor gain that was calculated by the evaluation unit 30 and normalizes with this value the sensor signal provided by the filter 26.
  • the senor signal can be made independent of gain variations.
  • the evaluation unit 30 may be used independently of the upper branch of the circuitry (which may therefore also miss).
  • the sensing current I 2 may be a direct current and the sensor gain may be measured in a separate procedure, stored and used later during real measurements for gain stabilization.

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  • Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Immunology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Pathology (AREA)
  • General Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Urology & Nephrology (AREA)
  • Hematology (AREA)
  • Biomedical Technology (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Molecular Biology (AREA)
  • Cell Biology (AREA)
  • Microbiology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Food Science & Technology (AREA)
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  • Dispersion Chemistry (AREA)
  • Measuring Magnetic Variables (AREA)
  • Investigating Or Analyzing Materials By The Use Of Magnetic Means (AREA)

Abstract

L'invention se rapporte à un biocapteur magnétique (10) comprenant un câble générateur de champ magnétique, et un élément capteur magnétique constitué d'un capteur à magnétorésistance géante (GMR) (12) activé par un courant de détection (12). Une unité d'évaluation (30) comprenant un filtre passe-bas (31), un amplificateur (32) et un circuit de traitement (33), mesure la proportion de bruit 1/f dans le signal de détection (UGMR), à partir de laquelle le gain du capteur peut être déterminé. Ledit gain du capteur peut être utilisé pour normaliser les mesures ordinaires du biocapteur (10), de façon à stabiliser ces mesures contre les variations de gain.
PCT/IB2007/050711 2006-03-15 2007-03-05 Capteur magnétique à stabilisation de gain Ceased WO2007105141A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP06111188 2006-03-15
EP06111188.6 2006-03-15

Publications (2)

Publication Number Publication Date
WO2007105141A2 true WO2007105141A2 (fr) 2007-09-20
WO2007105141A3 WO2007105141A3 (fr) 2008-03-06

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008075274A3 (fr) * 2006-12-18 2008-08-21 Koninkl Philips Electronics Nv Dispositif de détection magnétique avec traitement de signaux robustes
WO2008075262A3 (fr) * 2006-12-18 2008-08-21 Koninkl Philips Electronics Nv Dispositif de détection magnétique avec suppression de composantes de signal parasites
US20110194979A1 (en) * 2007-03-12 2011-08-11 Fabrico Technology, Inc. Modulated magnetic permeability sensing assays
US20110308330A1 (en) * 2010-06-21 2011-12-22 Lutz May Dynamic Signal Torque Sensor
JP2013083552A (ja) * 2011-10-11 2013-05-09 Hioki Ee Corp 電流センサ
CN103760222A (zh) * 2014-01-18 2014-04-30 中国矿业大学 一种基于巨磁电阻传感器阵列的矿用钢丝绳在线检测装置及方法
CN104359506A (zh) * 2014-11-06 2015-02-18 中国石油大学(北京) 用于钢缆生产质量监测的装置和方法
WO2020209964A1 (fr) 2019-04-12 2020-10-15 Western Digital Technologies, Inc. Capteurs à oscillateurs à couple de spin (sto) utilisés dans des réseaux de séquençage d'acides nucléiques et systèmes de détection pour le séquençage d'acides nucléiques
WO2020209911A1 (fr) 2019-04-12 2020-10-15 Western Digital Technologies, Inc. Réseau de capteurs magnétorésistifs pour la détection de molécules et schémas de détection associés
JP2020536220A (ja) * 2018-07-27 2020-12-10 ゼプト ライフ テクノロジー， エルエルシーＺｅｐｔｏ Ｌｉｆｅ Ｔｅｃｈｎｏｌｏｇｙ， Ｌｌｃ Ｇｍｒに基づくバイオマーカの検出における被検物質の信号を処理するシステムおよび方法

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US6437563B1 (en) * 1997-11-21 2002-08-20 Quantum Design, Inc. Method and apparatus for making measurements of accumulations of magnetically susceptible particles combined with analytes
US6875621B2 (en) * 1999-10-13 2005-04-05 Nve Corporation Magnetizable bead detector
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EP1525447A4 (fr) * 2002-05-31 2006-12-06 Univ California Procede et appareil de detection de substances d'interet
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KR20060054351A (ko) * 2003-07-30 2006-05-22 코닌클리케 필립스 일렉트로닉스 엔.브이. 개선된 신호대 잡음비를 가진 온칩 자기 입자 센서
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Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008075262A3 (fr) * 2006-12-18 2008-08-21 Koninkl Philips Electronics Nv Dispositif de détection magnétique avec suppression de composantes de signal parasites
WO2008075274A3 (fr) * 2006-12-18 2008-08-21 Koninkl Philips Electronics Nv Dispositif de détection magnétique avec traitement de signaux robustes
US8927260B2 (en) * 2007-03-12 2015-01-06 Fabrico Technology, Inc. Anaylte detection system using an oscillating magnetic field
US20110194979A1 (en) * 2007-03-12 2011-08-11 Fabrico Technology, Inc. Modulated magnetic permeability sensing assays
US20110308330A1 (en) * 2010-06-21 2011-12-22 Lutz May Dynamic Signal Torque Sensor
JP2013083552A (ja) * 2011-10-11 2013-05-09 Hioki Ee Corp 電流センサ
CN103760222A (zh) * 2014-01-18 2014-04-30 中国矿业大学 一种基于巨磁电阻传感器阵列的矿用钢丝绳在线检测装置及方法
CN104359506A (zh) * 2014-11-06 2015-02-18 中国石油大学(北京) 用于钢缆生产质量监测的装置和方法
JP2020536220A (ja) * 2018-07-27 2020-12-10 ゼプト ライフ テクノロジー， エルエルシーＺｅｐｔｏ Ｌｉｆｅ Ｔｅｃｈｎｏｌｏｇｙ， Ｌｌｃ Ｇｍｒに基づくバイオマーカの検出における被検物質の信号を処理するシステムおよび方法
WO2020209964A1 (fr) 2019-04-12 2020-10-15 Western Digital Technologies, Inc. Capteurs à oscillateurs à couple de spin (sto) utilisés dans des réseaux de séquençage d'acides nucléiques et systèmes de détection pour le séquençage d'acides nucléiques
WO2020209911A1 (fr) 2019-04-12 2020-10-15 Western Digital Technologies, Inc. Réseau de capteurs magnétorésistifs pour la détection de molécules et schémas de détection associés
EP3953703A4 (fr) * 2019-04-12 2022-06-08 Western Digital Technologies Inc. Réseau de capteurs magnétorésistifs pour la détection de molécules et schémas de détection associés
EP3953699A4 (fr) * 2019-04-12 2022-06-15 Western Digital Technologies Inc. Capteurs à oscillateurs à couple de spin (sto) utilisés dans des réseaux de séquençage d'acides nucléiques et systèmes de détection pour le séquençage d'acides nucléiques
US11738336B2 (en) 2019-04-12 2023-08-29 Western Digital Technologies, Inc. Spin torque oscillator (STO) sensors used in nucleic acid sequencing arrays and detection schemes for nucleic acid sequencing
US12241950B2 (en) 2019-04-12 2025-03-04 Western Digital Technologies, Inc. Magnetoresistive sensor array for molecule detection and related detection schemes

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