WO2004067797A1 - Arrangement consisting of a zinc oxide film applied to a substrate, method for producing said arrangement, and use of the same - Google Patents

Arrangement consisting of a zinc oxide film applied to a substrate, method for producing said arrangement, and use of the same Download PDF

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Publication number
WO2004067797A1
WO2004067797A1 PCT/EP2003/014342 EP0314342W WO2004067797A1 WO 2004067797 A1 WO2004067797 A1 WO 2004067797A1 EP 0314342 W EP0314342 W EP 0314342W WO 2004067797 A1 WO2004067797 A1 WO 2004067797A1
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Prior art keywords
zinc oxide
resonator
substrate
arrangement
oxide film
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PCT/EP2003/014342
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German (de)
French (fr)
Inventor
Reinhard Gabl
Matthias Schreiter
Bernd Utz
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Siemens Aktiengesellschaft
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Priority to AU2003290062A priority Critical patent/AU2003290062A1/en
Publication of WO2004067797A1 publication Critical patent/WO2004067797A1/en

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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3435—Applying energy to the substrate during sputtering
    • C23C14/3442—Applying energy to the substrate during sputtering using an ion beam
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
    • C30B23/02—Epitaxial-layer growth
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/16—Oxides
    • C30B29/22—Complex oxides
    • 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
    • G01N29/02—Analysing fluids
    • G01N29/036—Analysing fluids by measuring frequency or resonance of acoustic waves
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N30/00—Piezoelectric or electrostrictive devices
    • H10N30/01—Manufacture or treatment
    • H10N30/07—Forming of piezoelectric or electrostrictive parts or bodies on an electrical element or another base
    • H10N30/074—Forming of piezoelectric or electrostrictive parts or bodies on an electrical element or another base by depositing piezoelectric or electrostrictive layers, e.g. aerosol or screen printing
    • H10N30/076—Forming of piezoelectric or electrostrictive parts or bodies on an electrical element or another base by depositing piezoelectric or electrostrictive layers, e.g. aerosol or screen printing by vapour phase deposition
    • 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
    • G01N2291/01—Indexing codes associated with the measuring variable
    • G01N2291/014—Resonance or resonant frequency
    • 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
    • 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
    • G01N2291/0426—Bulk waves, e.g. quartz crystal microbalance, torsional waves
    • 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
    • G01N2291/10—Number of transducers
    • G01N2291/101—Number of transducers one transducer

Definitions

  • Zinc oxide film assembly on a substrate method of manufacturing the assembly and use of the assembly
  • the invention relates to an arrangement of a zinc oxide film on a substrate surface of a substrate, comprising a multiplicity of zinc oxide single crystals (zinc oxide crystallites), each with a [100] grating line (crystal axis), which is aligned essentially parallel to a surface normal of the substrate surface ,
  • a method for producing the arrangement and a use of the arrangement are specified.
  • the zinc oxide film of the arrangement is deposited on a quartz substrate by magnetron sputtering.
  • the deposited, polycrystalline zinc oxide film is characterized by three areas. In an outer area of the zinc oxide film, the [100] lattice lines of the zinc oxide single crystals of the zinc oxide film are aligned essentially parallel to the surface normal of the substrate surface. In an inner area of the zinc oxide film, the [002] lattice lines of the zinc oxide single crystals are aligned essentially parallel to the surface normal of the substrate surface. There is a transition region between the inner and the outer region, in which either the [100] -, the [002] - or the [101] lattice line of a zinc oxide single crystal is oriented essentially parallel to the surface normal.
  • the zinc oxide film of the known arrangement can form acoustic surface waves (surface acoustic waves, SAWs) or acoustic bulk waves (bulk acoustic waves, BAWs). be stimulated.
  • SAWs surface acoustic waves
  • BAWs bulk acoustic waves
  • BAW resonator bulk wave resonator
  • the zinc oxide film is arranged between two electrodes or electrode layers in such a way that a stacking sequence of substrate, first electrode layer, zinc oxide film and further electrode layer results along a stacking direction of the arrangement.
  • the zinc oxide film can be excited to longitudinal vibrations in the inner area parallel to the stacking direction and in the outer area to the thickness sensor vibration perpendicular to the stacking direction due to the orientation of the zinc oxide single crystals.
  • the arrangement described is characterized by a zinc oxide film which can be excited both to longitudinal vibrations and to thickness shear vibrations.
  • a zinc oxide film which can be excited both to longitudinal vibrations and to thickness shear vibrations.
  • HTS high temperature superconductivity
  • a polycrystalline metal oxide film In the field of high temperature superconductivity (HTS) it is known to use a polycrystalline metal oxide film. a certain texturing to grow on an amorphous substrate. A corresponding method can be seen, for example, from DE 199 32 444 Cl.
  • IBAD Ion Beam Assisted Deposition
  • the metal oxide film is deposited on the substrate by sputtering metal oxide from a sputtering target (evaporation source) by sputtering ions (for example argon ions, Ar + ).
  • the alignment of one of the crystallographic axes of the metal oxide single crystals perpendicular to the substrate surface is achieved.
  • a further crystallographic axis of each metal oxide single crystal is aligned in the film plane of the metal oxide film, that is to say perpendicular to the surface normal of the substrate surface.
  • the other crystallographic axes of the metal oxide single crystals are aligned parallel to one another.
  • the object of the present invention is to provide an arrangement made of a zinc oxide film on a substrate which can be designed to form an efficient piezoacoustic resonator.
  • the resonator should be able to be used in the presence of a liquid, with a damping of the resonator due to the liquid being smaller than in the prior art.
  • an arrangement consisting of a zinc oxide film on a substrate surface of a substrate comprising a multiplicity of zinc oxide single crystals, each with a [100] grid line, which is aligned essentially parallel to a surface normal of the substrate surface.
  • the arrangement is characterized in that the zinc oxide single crystals have [001] lattice lines which are aligned essentially parallel to one another.
  • Zinc oxide single crystals are essentially perpendicular to the given orientation of the [100] lattice line Surface normals of the substrate surface oriented.
  • the [100] grid lines have a common preferred direction.
  • the zinc oxide film is thus biaxially textured.
  • a method for producing the arrangement of the zinc oxide film on the substrate surface of the substrate by depositing zinc oxide on the substrate surface is also specified, with removal of zinc oxide and / or a precursor of the zinc oxide from a source of the Zinc oxide and / or the precursor of zinc oxide is carried out and during the deposition a beam of ions is directed obliquely onto the substrate surface of the substrate at a predetermined angle with respect to the surface normal of the substrate surface.
  • a so-called target is used as the source of the zinc oxide or the precursor of the zinc oxide.
  • the zinc oxide or the zinc oxide precursor can be removed from the target by means of an electron beam. According to a special one
  • a sputtering target is used as the source of the zinc oxide and / or the precursor of the zinc oxide, and a sputtering of the zinc oxide and / or the precursor of the zinc oxide from the sputtering target is carried out for removal by sputtering ions.
  • argon ions with an energy between 500 eV and 1500 eV are used as sputter ions.
  • the sputtering target can consist of zinc oxide.
  • a sputtering target made of elemental zinc is conceivable as a precursor of zinc oxide.
  • the elemental zinc is removed using sputter ions. In a reactive oxygen atmosphere, zinc oxide forms from this, which is deposited on the substrate surface.
  • the ions which are directed obliquely onto the substrate surface of the substrate are, for example, argon ions with an energy in the range of 100 eV to 1000 eV and in particular in the range of 200 eV to 500 eV.
  • the energy of the argon ions is 350 eV.
  • the angle of incidence of the ions or the beam from the ions is preferably selected from the range from 30 ° to 70 ° inclusive and in particular from the range from 40 ° to 60 ° inclusive. In a special embodiment, the angle of incidence is 58 °.
  • a polycrystalline zinc oxide film with biaxial texturing can be produced on a substrate.
  • the resulting arrangement can be configured into a BAW resonator for the excitation of thickness shear vibrations.
  • the crystallographic a-axis of a zinc oxide single crystal of the deposited zinc oxide film which corresponds to the [100] lattice line, is oriented essentially perpendicular to the substrate surface (parallel to the surface normal of the substrate surface).
  • the crystallographic c-axis of the zinc oxide single crystal which corresponds to the [001] lattice line, is aligned parallel to the substrate surface (perpendicular to the surface normal of the substrate surface).
  • the biaxial texturing results from the fact that the crystallographic c-axes of the zinc oxide single crystals are aligned essentially parallel to one another.
  • a substantially parallel alignment of the [100] grid lines of the zinc oxide single crystals to the surface normal of the substrate surface means that the [100] grid lines of the zinc oxide single crystals are oriented along a preferred direction parallel to the surface normal of the substrate surface.
  • the preferred direction can deviate from the exact parallelism to the surface normal by up to 20 °. However, the deviation is preferably below
  • the [100] lattice lines of the zinc oxide single crystals of the polycrystalline film can also differ from the preferred direction be aligned differently.
  • the [100] lattice lines of the single crystals with a half width of up to 20 ° can be distributed around this preferred direction.
  • the lattice lines of the zinc oxide-zinc oxide single crystals are essentially parallel to one another and thus aligned along a preferred direction.
  • the [001] grid lines can also be oriented differently from the preferred direction.
  • the [001] lattice lines of the single crystals with a half-value width of up to 20 ° can be distributed around this preferred direction.
  • the arrangement is preferably designed as a piezoacoustic resonator.
  • the piezoacoustic resonator can be designed as a surface wave resonator (SAW resonator).
  • the piezoacoustic resonator is preferably designed as a BAW resonator.
  • the arrangement has at least one electrode arranged on the zinc oxide film and at least one further electrode arranged on the zinc oxide film, the zinc oxide film and the electrodes being arranged to form a piezoacoustic resonator in such a way that electrical activation of the electrodes leads to a piezoacoustic oscillation of the resonator with a specific resonance frequency leads.
  • the electrodes are formed by electrode layers.
  • the zinc oxide film is arranged along the surface normal of the substrate surface between the electrode layers.
  • the arrangement has the stacking sequence of substrate, electrode layer, zinc oxide film and further electrode layer along a stacking direction. Due to the biaxial texturing, the resonator is primarily excited by the activation of the electrodes to vibrations of the thickness viewer perpendicular to the stacking direction.
  • the arrangement can be used to implement an acoustic
  • Frequency filters are used by which an electrical vibration of a certain frequency is damped.
  • Frequency filters bandpass filters and highpass or lowpass filters are conceivable.
  • the arrangement is used for the detection of a substance of a fluid.
  • the arrangement serves as a sensor of one or more chemical or biological substances.
  • the arrangement has a surface section which is chemically sensitive to a substance of a fluid, for sorption of the substance, the resonance frequency of the oscillation of the resonator being dependent on an amount of the substance which is sorbed on the chemically sensitive surface section.
  • the arrangement for detection is used with the following steps: a) bringing the fluid together and the arrangement such that the substance can be sorbed on the chemically sensitive surface section of the resonator and b) determining a resonance frequency of the resonator, the resonance frequency being based on the chemically sensitive surface section sorbed amount of the substance is closed.
  • the arrangement is designed as a BAW resonator, which functions as a so-called transducer (signal converter).
  • This transducer reacts to the amount of substance sorbed by changing the resonance frequency. The greater the amount of substance sorbed, the lower it is
  • Resonance frequency of the BAW resonator The following general relationship applies to the change in the resonance frequency ( ⁇ f) as a function of the change in the amount of substance sorbed per unit area ( ⁇ m) (compare G. Sauerbrey, Zeitschrift für Physik, 155 (1959), pp. 206-222):
  • a film thickness of the zinc oxide film is preferably selected from the range from 0.1 ⁇ m to 20 ⁇ m inclusive and the resonance frequency of the piezoacoustic oscillation of the resonator is selected from the range from 500 MHz to 10 GHz inclusive.
  • the arrangement is designed as a piezoacoustic thin film resonator.
  • a total layer thickness of the resonator consisting of electrode layers and zinc oxide film is, for example, 1 ⁇ m.
  • the mass of the resonator is relatively low. This increases the resonance frequency of the resonator.
  • the high resonance frequency results in a high mass sensitivity to the substance.
  • Mass sensitivity of the device can be estimated according to equation (1) to a few Hz-pg _1 -cm 2 .
  • the mass sensitivity at a resonance frequency of 1 GHz is approximately 2.5 Hz-pg -1 cm 2 .
  • the fluid with the substance can be a gas or gas mixture.
  • the arrangement is used for the detection of a substance of a fluid in the form of a liquid.
  • the arrangement in the form of the BAW resonator can be excited primarily to vibrate thick-sighted. In contrast to longitudinal vibrations, these thickness shear vibrations experience almost no damping due to a liquid that is in direct contact with the resonator. This means that the resonator can also be used in direct contact with the liquid.
  • the surface section is formed, for example, by a chemically sensitive coating of the arrangement. This coating ensures the sorption of the substance.
  • the chemically sensitive coating can be arranged on one or on both electrodes of the arrangement or the acoustic resonator.
  • the chemically sensitive Coating can also be applied directly to the zinc oxide film.
  • Sorption includes both absorption and adsorption.
  • the substance is absorbed, for example, by a coating of the resonator, which forms the surface section, without forming a phase boundary.
  • the substance is incorporated into the coating.
  • a phase boundary is formed during adsorption.
  • Adsorption in the form of physisorption is particularly conceivable.
  • the substance attaches to the surface section of the resonator through van der Waals or dipole-dipole interactions.
  • adsorption in the form of chemisorption can also take place.
  • the substance attaches to the surface section to form a chemical bond.
  • the chemical bond is, for example, a covalent bond or a hydrogen bond.
  • Sorption preferably takes place reversibly.
  • the substance can also be desorbed (removed) from the surface section.
  • the substance is removed by increasing the temperature of the surface portion ⁇ or by exposure to a reactive substance.
  • the reactive substance is, for example, an acid or an alkali, with the aid of which the bonds formed during chemisorption are released.
  • the device can be used several times in this way. It is also possible that the sorption is irreversible. The device is used only once as a disposable sensor.
  • the device can thus be designed as a biosensor for the detection of any biomolecule.
  • the biomolecule is, for example, a DNA (deoxynucleic acid) sequence or a macromolecular protein.
  • the chemical sensitive surface section or the chemically sensitive coating can also be designed for the adsorption of certain gaseous molecules.
  • gases are, for example, carbon monoxide, carbon dioxide, nitrogen oxides or sulfur oxides.
  • Low molecular weight organic gases such as methane or ethane are also conceivable
  • the surface section is preferably designed such that a specific substance or class of substances is selectively sorbed according to the keyhole principle. It is thus possible to selectively detect a specific substance from a mixture of a large number of substances with the aid of the arrangement.
  • the detection includes both a qualitative and quantitative determination of the substance.
  • each of the resonators described are combined to form a resonator matrix and each of the resonators forms a matrix element of the resonator matrix.
  • each resonator is designed in such a way that it is sensitive to a specific substance or class of substances. In this way, the arrangement of substance can be analyzed qualitatively and / or quantitatively.
  • one of the resonators is sensitive to hydrocarbons
  • a second resonator is sensitive to sulfur oxides
  • another resonator is sensitive to carbon monoxide.
  • each of the resonators of the individual matrix elements is sensitive to a specific DNA sequence. The presence of different DNA sequences in a fluid can thus be examined in parallel.
  • the resonator can be arranged on any substrate.
  • the substrate is preferably characterized by a material with a low loss for high-frequency signals. Such a material is, for example, sapphire.
  • the zinc oxide film is arranged on a substrate made of a semiconductor material.
  • the semiconductor material is preferably selected from the group consisting of silicon and / or gallium arsenide.
  • the substrate can be single crystal or polycrystalline.
  • the semiconductor materials mentioned are suitable for the use of bipolar and CMOS (Complementary Metal Oxide Semiconductor) technology for integrating control and / or evaluation devices of the resonator.
  • the arrangement preferably has at least one device for acoustically isolating the resonator and the substrate.
  • the resonator and the substrate are acoustically isolated from each other.
  • the acoustic insulation ensures that the resonance frequency of the resonator is independent of the substrate.
  • the result is a relatively high mass sensitivity.
  • the device for acoustic isolation is, for example, a Bragg reflector, which consists of ⁇ / 4 thick layers of different acoustic impedance.
  • the device is formed by a cavity in the substrate.
  • a biaxially textured, polycrystalline zinc oxide film is accessible on any substrate.
  • the zinc oxide film is homogeneous. This means that the entire film can be biaxially textured in the thickness direction as well as along a lateral dimension.
  • the zinc oxide single crystals are preferably oriented in such a way that the zinc oxide film as part of a BAW resonator can essentially only be excited to vibrate in thickness.
  • the BAW Resonator can be without strong damping
  • Resonance frequency can be used in direct contact with a liquid.
  • the arrangement can be designed for the detection of a substance.
  • the arrangement is characterized by a high mass sensitivity.
  • Figure la shows an arrangement of a zinc oxide film on a substrate surface of a substrate in
  • Figure lb shows the arrangement in plan view of the zinc oxide film.
  • Figure 2 shows an arrangement in the form of a biosensor.
  • Figure 3 shows an arrangement with several biosensors in cross section.
  • FIG. 4 shows a method for detecting a substance
  • FIG. 5 shows a method for producing the zinc oxide film.
  • the arrangement 1 consists of a polycrystalline zinc oxide film 2 on a substrate 3 made of silicon ( Figures la and lb).
  • the zinc oxide film 2 is applied to a substrate surface 4 of the substrate 3.
  • the zinc oxide film 2 consists of a large number of zinc oxide single crystals.
  • Grid lines of the individual zinc oxide single crystals have an orientation 6 in the direction of the surface normal 5 of the Substrate surface 4.
  • the grating lines of the zinc oxide single crystals are parallel to one another and aligned along the substrate surface 4. [001]
  • the grid lines have an orientation 7 perpendicular to the surface normal 5. In this constellation, the zinc oxide film 2 can be excited to give thickness shear vibrations 12 along the lateral extent 17 of the zinc oxide film 2.
  • the IBAD method is used to produce the zinc oxide film 2 on the substrate 3 (FIG. 5). It is in one
  • Sputter chamber 101 deposited the zinc oxide on the substrate surface 4 of the substrate 3.
  • the sputtering chamber 101 has an oxygen atmosphere.
  • zinc oxide is sputtered (evaporated) from a sputtering target 102 made of zinc oxide by sputtering ions 103.
  • the sputterions are
  • Argon ions with an energy between 500 eV and 1500 eV. These argon ions are generated by an ion source 106 and directed onto the sputtering target 102.
  • the sputtering ions 103 strike the sputtering target 102 at an angle and release zinc oxide particles 107 there from the surface of the sputtering target 102.
  • These zinc oxide particles 107 reach the substrate 3 arranged opposite the sputtering target 102 and are deposited there on the substrate surface 4 of the substrate 3.
  • an assisting beam of ions 104 is directed obliquely onto the substrate surface 4 of the substrate 3 at a predetermined angle of incidence 105 with respect to the surface normal 5 of the substrate surface 4.
  • the angle of incidence is 58 °.
  • the ions 104 are argon ions with an energy of approximately 350 eV. These argon ions are generated by a further ion source 108 and directed onto the substrate surface 4.
  • the arrangement 1 is used for the detection of a substance.
  • the arrangement 1 is configured as a piezoacoustic resonator (BAW resonator) 10 which is based on a Semiconductor substrate 3 made of silicon is applied ( Figure 2).
  • the resonator 10 has the piezoelectrically active zinc oxide film 2.
  • the film thickness 11 of the zinc oxide film is approximately 0.8 ⁇ m.
  • the lateral extent 17 of the resonator 10 is approximately 100 ⁇ m.
  • the electrodes 8 and 9 are arranged in the form of electrode layers on two sides of the zinc oxide film 2 facing away from one another.
  • the layer thickness of the electrode layers 8 and 9 is in each case approximately 0.1 ⁇ m.
  • the electrodes 8 and 9 are off
  • An electrical insulation 18 made of aluminum oxide additionally separates the electrodes 8 and 9.
  • the resonator 10 is excited to the thickness shear vibrations 12 by electrical control of the electrodes 8 and 9.
  • the resonator 10 has a surface section 13 on which a substance of a fluid 15 can be sorbed.
  • the resonator 10 has a chemically sensitive coating 14.
  • the chemically sensitive coating 14 is applied to the electrode 8.
  • the semiconductor substrate 3 and the resonator 10 are acoustically isolated from one another with the aid of a device for acoustic isolation 16.
  • the device 16 is a Bragg reflector with ⁇ / 4 thick layers of different impedance.
  • FIG. 3 shows a device 1 with three resonators 10 in a lateral cross section.
  • the resonators 10 are applied to a semiconductor substrate 3 made of silicon to form a resonator matrix 19.
  • the resonators 10 each form a matrix element 20 of the resonator matrix 19.
  • Each of the resonators 10 has a lateral dimension 17 of approximately 100 ⁇ m.
  • a distance 21 between adjacent matrix elements 20 is 100 ⁇ m.
  • Each of the matrix elements 21 has a resonator 10 sensitive to a specific substance.
  • the arrangement is used for the detection of a substance of a fluid 15 in the form of a liquid.
  • the chemically sensitive surface section 13 of the resonator 10 and the fluid 15 are brought together in a first step (FIG. 4, step 41).
  • the fluid 15 and the resonator 10 are brought together in such a way that the substance of the fluid 15 can be sorbed on the respective surface sections 13 of the resonator 10.
  • the mass of the resonator 10 changes as a result of the sorption.
  • the type of substance and its concentration in the fluid 15 can be inferred from subsequent measurement of the resonance frequencies of the resonator 10 (FIG. 4, step 42).
  • the sorption of the substance changes the resonance frequency of the resonator 10 compared to the resonance frequency of the resonator 10, on the surface section 13 of which no substance is sorbed.
  • a resonator 10 with a known resonance frequency is used.
  • the resonance frequency of the resonator without the sorbed substance is determined before the fluid and the resonator are brought together.

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Abstract

The invention relates to an arrangement (1) consisting of a zinc oxide film (2) applied to the surface (4) of a substrate (3), said arrangement comprising a plurality of zinc oxide monocrystals respectively having a [100] lattice line which is oriented essentially parallel to a normal (5) of the substrate surface. The arrangement is characterised in that the zinc oxide monocrystals respectively have a [001] lattice line which is essentially perpendicular to the normal of the substrate surface, and the [001] lattice lines of the zinc oxide monocrystals are essentially parallel to each other. According to the invention, the IBAD (Ion Beam Assisted Deposition) method is used to produce one such arrangement. In this way, zinc oxide or a precursor of the zinc oxide is removed, especially sputtered by a target, especially a sputtering target, for the deposition, and during the deposition, an ion beam is obliquely directed towards the surface of the substrate at a pre-determined angle of incidence in relation to the normal of the substrate surface. The resulting zinc oxide film is biaxially textured. When the inventive arrangement is in the form of a bulk acoustic wave resonator (BAW resonator), the zinc oxide film is excited in such a way that thickness shear vibrations are generated as a result of the texturing. The resonator is used as the transducer of a biosensor.

Description

Anordnung aus einem Zinkoxidfilm auf einem Substrat, Verfahren zum Herstellen der Anordnung und Verwendung der AnordnungZinc oxide film assembly on a substrate, method of manufacturing the assembly and use of the assembly
Die Erfindung betrifft eine Anordnung aus einem Zinkoxidfilm auf einer Substratoberfläche eines Substrats, aufweisend eine Vielzahl von Zinkoxid-Einkristallen (Zinkoxid-Kristallite)mit jeweils einer [100] -Gittergeraden (-Kristallache), die im Wesentlichen parallel zu einer Flächennormalen der Substratoberfläche ausgerichtet ist. Daneben wird ein Verfahren zum Herstellen der Anordnung und eine Verwendung der Anordnung angegeben.The invention relates to an arrangement of a zinc oxide film on a substrate surface of a substrate, comprising a multiplicity of zinc oxide single crystals (zinc oxide crystallites), each with a [100] grating line (crystal axis), which is aligned essentially parallel to a surface normal of the substrate surface , In addition, a method for producing the arrangement and a use of the arrangement are specified.
Eine derartige Anordnung und ein derartiges Verfahren zum Herstellen der Anordnung sind aus A. G. Veselov et al . , Technical Physics, Vol. 45, No . 4 (2000), Seiten 497-500 bekannt. Der Zinkoxidfilm der Anordnung wird durch Magnetron- Sputtern auf einem Substrat aus Quarz abgeschieden. Der dabei abgeschiedene, polykristalline Zinkoxidfilm zeichnet sich durch drei Bereiche aus . In einem äußeren Bereich des Zinkoxidfilms sind die [100] -Gittergeraden der Zinkoxid- Einkristalle des Zinkoxidfilms im Wesentlichen parallel zur Flächennormalen der Substratoberfläche ausgerichtet. In einem inneren Bereich des Zinkoxidfilms sind die [002]- Gittergeraden der Zinkoxid-Einkristalle im Wesentlichen parallel zur Flächennormalen der Substratoberfläche ausgerichtet. Zwischen dem inneren und dem äußeren Bereich gibt es einen Übergangsbereich, in dem entweder die [100]-, die [002]- oder die [101] -Gittergerade eines Zinkoxid- Einkristalls im Wesentlichen parallel zur Flächennormalen ausgerichtet ist.Such an arrangement and such a method for producing the arrangement are known from A.G. Veselov et al. , Technical Physics, Vol. 45, No. 4 (2000), pages 497-500. The zinc oxide film of the arrangement is deposited on a quartz substrate by magnetron sputtering. The deposited, polycrystalline zinc oxide film is characterized by three areas. In an outer area of the zinc oxide film, the [100] lattice lines of the zinc oxide single crystals of the zinc oxide film are aligned essentially parallel to the surface normal of the substrate surface. In an inner area of the zinc oxide film, the [002] lattice lines of the zinc oxide single crystals are aligned essentially parallel to the surface normal of the substrate surface. There is a transition region between the inner and the outer region, in which either the [100] -, the [002] - or the [101] lattice line of a zinc oxide single crystal is oriented essentially parallel to the surface normal.
Der Zinkoxidfilm der bekannten Anordnung kann zu akustischen Oberflächenwellen (Surface Acoustic Waves, SAWs) oder zu akustischen Volumenwellen (Bulk Acoustic Waves, BAWs) angeregt werden. Zur Anregung von akustischen Volumenwellen ist die Anordnung als Volumenwellen-Resonator (BAW-Resonator) ausgestaltet. Dabei wird der Zinkoxidfilm zwischen zwei Elektroden bzw. Elektrodenschichten derart angeordnet, dass eine Stapelfolge aus Substrat, erste Elektrodenschicht, Zinkoxidfilm und weitere Elektrodenschicht entlang einer Stapelrichtung der Anordnung resultiert. Durch Ansteuerung der Elektroden kann der Zinkoxidfilm aufgrund der Orientierung der Zinkoxid-Einkristalle im inneren Bereich zu Längsschwingungen parallel zur Stapelrichtung und im äußeren Bereich zu DickenseherSchwingung senkrecht zur Stapelrichtung angeregt werden.The zinc oxide film of the known arrangement can form acoustic surface waves (surface acoustic waves, SAWs) or acoustic bulk waves (bulk acoustic waves, BAWs). be stimulated. To excite bulk acoustic waves, the arrangement is designed as a bulk wave resonator (BAW resonator). The zinc oxide film is arranged between two electrodes or electrode layers in such a way that a stacking sequence of substrate, first electrode layer, zinc oxide film and further electrode layer results along a stacking direction of the arrangement. By activating the electrodes, the zinc oxide film can be excited to longitudinal vibrations in the inner area parallel to the stacking direction and in the outer area to the thickness sensor vibration perpendicular to the stacking direction due to the orientation of the zinc oxide single crystals.
Die beschriebene Anordnung zeichnet sich durch einen Zinkoxidfilm aus, der sowohl zu LängsSchwingungen als auch zu Dickenscherschwingungen angeregt werden kann. Insbesondere bei der Verwendung der Anordnung als BAW-Resonator in Gegenwart einer Flüssigkeit kann es aber zu einer unterwünschten Dämpfung der LängsSchwingung des Zinkoxidfilms bzw. des Resonators kommen.The arrangement described is characterized by a zinc oxide film which can be excited both to longitudinal vibrations and to thickness shear vibrations. In particular, when the arrangement is used as a BAW resonator in the presence of a liquid, undesired damping of the longitudinal vibration of the zinc oxide film or of the resonator can occur.
Auf dem Gebiet der Hochtemperatursupraleitung (HTS) ist es bekannt, einen polykristallinen Metalloxid-Film mit. einer bestimmten Texturierung auf einem amorphen Substrat aufwachsen zu lassen. Ein entsprechendes Verfahren geht beispielsweise aus der DE 199 32 444 Cl hervor. Dieses Verfahren basiert auf einem speziellen Abscheideverfahren, das als Ion Beam Assisted Deposition (IBAD) bekannt ist. Der Metalloxid-Film wird durch ein Absputtern von Metalloxid von einem Sputtertarget (Verdampfungsquelle) durch Sputterionen (beispielsweise Argonionen, Ar+) auf dem Substrat abgeschieden. Während des Abscheidens wird dabei ein Strahl ■ von Ionen (beispielsweise Ar+) schräg auf die Substratoberfläche unter einem vorbestimmten Einfallswinkel bezüglich der Flächennormalen der Substratoberfläche gerichtet. Mit Hilfe dieses IBÄD-Verfahr.ens ist es möglich, den Metalloxid-Film mit biaxialer Texturierung auf der Substratoberfläche abzuscheiden. Unter Texturierung wird die Ausrichtung der Metalloxid-Einkristalle des Metalloxid-Films in einem entsprechenden polykristallinen Gefüge verstanden. Bei einer biaxialen Texturierung sind die Metalloxid- Einkristalle derart ausgerichtet, dass zwei der kristallographischen Achsen der Metalloxid-Einkristalle jeweils eine Vorzugsrichtung aufweisen. Mit dem aus der DE 199 32 444 Cl bekannten IBAD-Verfahren wird die Ausrichtung einer der kristallographischen Achsen der Metalloxid- Einkristalle senkrecht zur Substratoberfläche (parallel zur Flächennormalen der Substratoberfläche) erreicht. Zusätzlich ist eine weitere kristallographische Achse eines jeden Metalloxid-Einkristalls in der Filmebene des Metalloxid- Films, also senkrecht zur Flächennormalen der Substratoberfläche ausgerichtet. Dabei sind die weiteren kristallographischen Achsen der Metalloxid-Einkristalle zueinander parallel ausgerichtet. •In the field of high temperature superconductivity (HTS) it is known to use a polycrystalline metal oxide film. a certain texturing to grow on an amorphous substrate. A corresponding method can be seen, for example, from DE 199 32 444 Cl. This process is based on a special deposition process known as Ion Beam Assisted Deposition (IBAD). The metal oxide film is deposited on the substrate by sputtering metal oxide from a sputtering target (evaporation source) by sputtering ions (for example argon ions, Ar + ). During the deposition, while a beam of ions ■ (for example, Ar +) obliquely to the substrate surface at a predetermined incident angle relative to the surface normal of the substrate surface is directed. With the help of this IBÄD process, it is possible to biaxially texturize the metal oxide film on the Deposit substrate surface. Texturing is understood to mean the alignment of the metal oxide single crystals of the metal oxide film in a corresponding polycrystalline structure. In the case of biaxial texturing, the metal oxide single crystals are aligned in such a way that two of the crystallographic axes of the metal oxide single crystals each have a preferred direction. With the IBAD method known from DE 199 32 444 C1, the alignment of one of the crystallographic axes of the metal oxide single crystals perpendicular to the substrate surface (parallel to the surface normal of the substrate surface) is achieved. In addition, a further crystallographic axis of each metal oxide single crystal is aligned in the film plane of the metal oxide film, that is to say perpendicular to the surface normal of the substrate surface. The other crystallographic axes of the metal oxide single crystals are aligned parallel to one another. •
Aufgabe der vorliegenden Erfindung ist es, eine Anordnung aus einem Zinkoxidfilm auf einem Substrat anzugeben, die zu einem effizienten piezoakustischen Resonator ausgestaltet werden kann. Der Resonator soll dabei in Gegenwart einer Flüssigkeit verwendet werden können, wobei eine Dämpfung des Resonators aufgrund der Flüssigkeit im Vergleich zum Stand der Technik kleiner sein soll.The object of the present invention is to provide an arrangement made of a zinc oxide film on a substrate which can be designed to form an efficient piezoacoustic resonator. The resonator should be able to be used in the presence of a liquid, with a damping of the resonator due to the liquid being smaller than in the prior art.
Zur Lösung der Aufgabe wird eine Anordnung aus einem Zinkoxidfilm auf einer Substratoberfläche eines Substrats angegeben, aufweisend eine Vielzahl von Zinkoxid- Einkristallen mit jeweils einer [100] -Gittergeraden, die im Wesentlichen parallel zu einer Flächennormalen der Substratoberfläche ausgerichtet ist. Die Anordnung ist dadurch gekennzeichnet, dass die Zinkoxid-Einkristalle [001]- Gittergeraden aufweisen, die im Wesentlichen zueinander parallel ausgerichtet sind. Die [001] -Gittergeraden derTo achieve the object, an arrangement consisting of a zinc oxide film on a substrate surface of a substrate is specified, comprising a multiplicity of zinc oxide single crystals, each with a [100] grid line, which is aligned essentially parallel to a surface normal of the substrate surface. The arrangement is characterized in that the zinc oxide single crystals have [001] lattice lines which are aligned essentially parallel to one another. The [001] grid lines of the
Zinkoxid-Einkristalle sind durch die vorgegebene Orientierung der [100] -Gittergeraden im Wesentlichen senkrecht zur Flächennormalen der Substratoberfläche orientiert. Darüber hinaus weisen die [100] -Gittergeraden eine gemeinsame Vorzugsrichtung auf. Der Zinkoxid-Film ist somit biaxial texturiert.Zinc oxide single crystals are essentially perpendicular to the given orientation of the [100] lattice line Surface normals of the substrate surface oriented. In addition, the [100] grid lines have a common preferred direction. The zinc oxide film is thus biaxially textured.
Zur Lösung der Aufgabe wird auch ein Verfahren zum Herstellen der Anordnung des Zink-Oxid-Films auf der Substratoberfläche des Substrats durch Abscheiden von Zinkoxid auf der Substratoberfläche angegeben, wobei zum Abscheiden ein Abtragen von Zinkoxid und/oder einer Vorstufe des Zinkoxids von einer Quelle des Zinkoxids und/oder der Vorstufe des Zinkoxids durchgeführt wird und während des Abscheidens ein Strahl von Ionen schräg auf die Substratoberfläche des Substrats unter einem vorbestimmten Ein allswinkel bezüglich der Flächennormalen der Substratoberfläche gerichtet wird.To achieve the object, a method for producing the arrangement of the zinc oxide film on the substrate surface of the substrate by depositing zinc oxide on the substrate surface is also specified, with removal of zinc oxide and / or a precursor of the zinc oxide from a source of the Zinc oxide and / or the precursor of zinc oxide is carried out and during the deposition a beam of ions is directed obliquely onto the substrate surface of the substrate at a predetermined angle with respect to the surface normal of the substrate surface.
Als Quelle des Zinkoxids oder der Vorstufe des Zinkoxid wird ein sogenanntes Target verwendet. Das Abtragen des Zinkoxids oder der Vorstufe des Zinkoxids vom Targen kann durch einen Elektronenstrahl erfolgen. Gemäß einer besonderenA so-called target is used as the source of the zinc oxide or the precursor of the zinc oxide. The zinc oxide or the zinc oxide precursor can be removed from the target by means of an electron beam. According to a special one
Ausgestaltung wird als Quelle des Zinkoxids und/oder der Vorstufe des Zinkoxids ein Sputtertarget verwendet und zum Abtragen ein Absputtern des Zinkoxid und/oder der Vorstufe des Zinkoxids von dem Sputtertarget durch Sputterionen durchgeführt .A sputtering target is used as the source of the zinc oxide and / or the precursor of the zinc oxide, and a sputtering of the zinc oxide and / or the precursor of the zinc oxide from the sputtering target is carried out for removal by sputtering ions.
Als Sputterionen werden beispielsweise Argonionen mit einer Energie zwischen 500 eV und 1500 eV verwendet. Das Sputtertarget kann aus Zinkoxid bestehen. Als Vorstufe des Zinkoxids ist beispielsweise ein Sputtertarget aus elementarem Zink denkbar. Das elementare Zink wird mit Hilfe der Sputterionen abgetragen. In einer reaktiven Sauerstoffatmosphäre bildet sich daraus Zinkoxid, das auf der Substratoberfläche abgeschieden wird.For example, argon ions with an energy between 500 eV and 1500 eV are used as sputter ions. The sputtering target can consist of zinc oxide. For example, a sputtering target made of elemental zinc is conceivable as a precursor of zinc oxide. The elemental zinc is removed using sputter ions. In a reactive oxygen atmosphere, zinc oxide forms from this, which is deposited on the substrate surface.
Die Ionen, die schräg auf die -Substratoberfläche des Substrats gerichtet werden, sind beispielsweise Argonionen mit einer Energie aus dem Bereich von 100 eV bis 1000 eV und insbesondere aus dem Bereich von 200 eV bis 500 eV. Beispielsweise beträgt die Energie der Argonionen 350 eV. Der Einfallswinkel der Ionen bzw. des Strahls aus den Ionen wird vorzugsweise aus dem Bereich von einschließlich 30° bis einschließlich 70° und insbesondere aus dem Bereich von einschließlich 40° bis einschließlich 60° ausgewählt. In einer besonderen Ausgestaltung beträgt der Einfallswinkel 58°. Mit Hilfe des Verfahrens gelingt es, einen polykristallinen Zinkoxidfilm mit biaxialer Texturierung auf einem Substrat herzustellen. Die daraus resultierende Anordnung kann zu einem BAW-Resonator zur Anregung von Dickenscherschwingungen ausgestaltet werden.The ions which are directed obliquely onto the substrate surface of the substrate are, for example, argon ions with an energy in the range of 100 eV to 1000 eV and in particular in the range of 200 eV to 500 eV. For example, the energy of the argon ions is 350 eV. The angle of incidence of the ions or the beam from the ions is preferably selected from the range from 30 ° to 70 ° inclusive and in particular from the range from 40 ° to 60 ° inclusive. In a special embodiment, the angle of incidence is 58 °. With the help of the process, a polycrystalline zinc oxide film with biaxial texturing can be produced on a substrate. The resulting arrangement can be configured into a BAW resonator for the excitation of thickness shear vibrations.
Die kristallographische a-Achse eines Zinkoxid-Einkristalls des abgeschiedenen Zinkoxid-Films, die der [100]- Gittergeraden entspricht, ist im Wesentlichen senkrecht zur Substratoberfläche (parallel zur Flächennormale der Substratoberfläche) ausgerichtet. Als Konsequenz daraus ist die kristallographische c-Achse des Zinkoxid-Einkristalls, die der [001] -Gittergeraden entspricht, parallel zur Substratoberflache ausgerichtet (senkrecht zur Flächennormale des Substratoberfläche) . Die biaxiale Texturierung ergibt sich daraus, dass die kristallographischen c-Achsen der Zinkoxid-Einkristalle zueinander im Wesentlichen parallel ausgerichtet sind.The crystallographic a-axis of a zinc oxide single crystal of the deposited zinc oxide film, which corresponds to the [100] lattice line, is oriented essentially perpendicular to the substrate surface (parallel to the surface normal of the substrate surface). As a consequence, the crystallographic c-axis of the zinc oxide single crystal, which corresponds to the [001] lattice line, is aligned parallel to the substrate surface (perpendicular to the surface normal of the substrate surface). The biaxial texturing results from the fact that the crystallographic c-axes of the zinc oxide single crystals are aligned essentially parallel to one another.
Eine im Wesentlichen parallele Ausrichtung der [100]- Gittergeraden der Zinkoxid-Einkristalle zur Flächennormalen der Substratoberfläche bedeutet, dass die [100] -Gittergeraden der Zinkoxid-Einkristalle entlang einer Vorzugsrichtung parallel zur Flächennormalen der Substratoberfläche orientiert sind. Die Vorzugsrichtung kann dabei von der exakten Parallelität zur Flächennormalen um bis zu 20° abweichen. Die Abweichung beträgt aber vorzugsweise unterA substantially parallel alignment of the [100] grid lines of the zinc oxide single crystals to the surface normal of the substrate surface means that the [100] grid lines of the zinc oxide single crystals are oriented along a preferred direction parallel to the surface normal of the substrate surface. The preferred direction can deviate from the exact parallelism to the surface normal by up to 20 °. However, the deviation is preferably below
10°. Die [100] -Gittergeraden der Zinkoxid-Einkristalle des polykristallinen Films können zudem von der Vorzugsrichtung abweichend ausgerichtet sein. Um diese Vorzugsrichtung können die [100] -Gittergeraden der Einkristalle mit einer Halbwertsbreite von bis zu 20° verteilt sein.10 °. The [100] lattice lines of the zinc oxide single crystals of the polycrystalline film can also differ from the preferred direction be aligned differently. The [100] lattice lines of the single crystals with a half width of up to 20 ° can be distributed around this preferred direction.
Die [001] -Gittergeraden der Zinkoxid-Zinkoxid-Einkristalle sind im Wesentlichen parallel zueinander und damit entlang einer Vorzugsrichtung ausgerichtet. Auch die [001]- Gittergeraden können von der Vorzugsrichtung abweichend ausgerichtet sein. Um diese Vorzugsrichtung können die [001]- Gittergeraden der Einkristalle mit einer Halbwertsbreite von bis zu 20° verteilt sein.The lattice lines of the zinc oxide-zinc oxide single crystals are essentially parallel to one another and thus aligned along a preferred direction. The [001] grid lines can also be oriented differently from the preferred direction. The [001] lattice lines of the single crystals with a half-value width of up to 20 ° can be distributed around this preferred direction.
Die Anordnung ist bevorzugt als piezoakustischer Resonator ausgestaltet. Der piezoakustische Resonator kann dabei als Oberflächenwellen-Resonator (SAW-Resonator) ausgestaltet sein. Vorzugsweise ist der piezoakustische Resonator als BAW- Resonator ausgestaltet. Dazu weist die Anordnung mindestens eine am Zinkoxidfilm angeordnete Elektrode und mindestens eine am Zinkoxidfilm angeordnete weitere Elektrode auf, wobei der Zinkoxidfilm und die Elektroden derart zu einem piezoakustischen Resonator angeordnet sind, dass eine elektrische Ansteuerung der Elektroden zu einer piezoakustischen Schwingung des Resonators mit einer bestimmten Resonanzfrequenz führt. Die Elektroden werden von Elektrodenschichten gebildet. Der Zinkoxidfilm ist entlang der Flächennormalen der Substratoberfläche zwischen den Elektrodenschichten angeordnet. Die Anordnung weist entlang einer Stapelrichtung die Stapelfolge aus Substrat, Elektrodenschicht, Zinkoxidfilm und weitere Elektrodenschicht auf. Durch die biaxiale Texturierung wird der Resonator durch die Ansteuerung der Elektroden in erster Linie zu Dickenseherschwingungen- senkrecht zur Stapelrichtung angeregt .The arrangement is preferably designed as a piezoacoustic resonator. The piezoacoustic resonator can be designed as a surface wave resonator (SAW resonator). The piezoacoustic resonator is preferably designed as a BAW resonator. For this purpose, the arrangement has at least one electrode arranged on the zinc oxide film and at least one further electrode arranged on the zinc oxide film, the zinc oxide film and the electrodes being arranged to form a piezoacoustic resonator in such a way that electrical activation of the electrodes leads to a piezoacoustic oscillation of the resonator with a specific resonance frequency leads. The electrodes are formed by electrode layers. The zinc oxide film is arranged along the surface normal of the substrate surface between the electrode layers. The arrangement has the stacking sequence of substrate, electrode layer, zinc oxide film and further electrode layer along a stacking direction. Due to the biaxial texturing, the resonator is primarily excited by the activation of the electrodes to vibrations of the thickness viewer perpendicular to the stacking direction.
Die Anordnung kann zur Realisierung eines akustischenThe arrangement can be used to implement an acoustic
Frequenzfilters verwendet werden, durch das eine elektrische Schwingung einer bestimmten Frequenz gedämpft wird. Als Frequenzfilter sind dabei Bandpassfilter sowie Hochpass- oder Tiefpassfilter denkbar.Frequency filters are used by which an electrical vibration of a certain frequency is damped. As Frequency filters, bandpass filters and highpass or lowpass filters are conceivable.
Insbesondere wird die Anordnung zur Detektion einer Substanz eines Fluids verwendet. Die Anordnung dient als Sensor einer oder mehrerer chemischer oder biologischer Substanzen. Die Anordnung weist dazu einen gegenüber einer Substanz eines Fluids chemisch sensitiven Oberflächenabschnitt zur Sorption der Substanz auf, wobei die Resonanzfrequenz der Schwingung des Resonators abhängig ist von einer Menge der Substanz, die auf dem chemisch sensitiven Oberflächenabschnitt sorbiert ist. Die Verwendung der Anordnung zur Detektion erfolgt dabei mit den Schritten: a) Zusammenbringen des Fluids und der Anordnung derart, dass die Substanz am chemisch sensitiven Oberflächenabschnitt des Resonators sorbiert werden kann und b) Bestimmen einer Resonanzfrequenz des Resonators, wobei aus der Resonanzfrequenz auf die am chemisch sensitiven Oberflächenabschnitt sorbierte Menge der Substanz geschlossen wird.In particular, the arrangement is used for the detection of a substance of a fluid. The arrangement serves as a sensor of one or more chemical or biological substances. For this purpose, the arrangement has a surface section which is chemically sensitive to a substance of a fluid, for sorption of the substance, the resonance frequency of the oscillation of the resonator being dependent on an amount of the substance which is sorbed on the chemically sensitive surface section. The arrangement for detection is used with the following steps: a) bringing the fluid together and the arrangement such that the substance can be sorbed on the chemically sensitive surface section of the resonator and b) determining a resonance frequency of the resonator, the resonance frequency being based on the chemically sensitive surface section sorbed amount of the substance is closed.
Die Anordnung ist zu einem BAW-Resonator ausgebildet, der als sogenannter Transduktor (Signalwandler) fungiert. Dieser Transduktor reagiert auf die sorbierte Menge der Substanz mit einer Änderung der Resonanzfrequenz. Je größer die sorbierte Menge der Substanz ist, desto niedriger ist dieThe arrangement is designed as a BAW resonator, which functions as a so-called transducer (signal converter). This transducer reacts to the amount of substance sorbed by changing the resonance frequency. The greater the amount of substance sorbed, the lower it is
Resonanzfrequenz des BAW-Resonators . Für die Änderung der Resonanzfrequenz (Δf) in Abhängigkeit von der Änderung der sorbierten Menge der Substanz pro Flächeneinheit (Δm) gilt folgender allgemeine Zusammenhang (vergleiche G. Sauerbrey, Zeitschrift für Physik, 155 (1959), S. 206 - 222):Resonance frequency of the BAW resonator. The following general relationship applies to the change in the resonance frequency (Δf) as a function of the change in the amount of substance sorbed per unit area (Δm) (compare G. Sauerbrey, Zeitschrift für Physik, 155 (1959), pp. 206-222):
S = - = C£- rf (1)S = - = C £ - rf (1)
Δm mΔm m
Dabei ist S die Massensensitivität des Resonators, f0 die Resonanzfrequenz des Resonators ohne adsorbierte Substanz, c ist eine materialspezifische Konstante und m die Masse des Resonators pro Flächeneinheit. Die Massensensitivität ist proportional zum Quadrat der Resonanzfrequenz des Resonators. Vorzugsweise ist daher eine Filmdicke des Zinkoxidfilms aus dem Bereich von einschließlich 0,1 μm bis einschließlich 20 • μm und die Resonanzfrequenz der piezoakustischen Schwingung des Resonators aus dem Bereich von einschließlich 500 MHz bis einschließlich 10 GHz ausgewählt. Die Anordnung ist als piezoakustischer Dünnfilmresonator ausgestaltet. Eine Gesamtschichtdicke des Resonators aus Elektrodenschichten und Zinkoxidfilm beträgt beispielsweise 1 μm. Durch die kleineS is the mass sensitivity of the resonator, f 0 is the resonance frequency of the resonator without adsorbed substance, c is a material-specific constant and m is the mass of the Resonators per unit area. The mass sensitivity is proportional to the square of the resonance frequency of the resonator. Therefore, a film thickness of the zinc oxide film is preferably selected from the range from 0.1 μm to 20 μm inclusive and the resonance frequency of the piezoacoustic oscillation of the resonator is selected from the range from 500 MHz to 10 GHz inclusive. The arrangement is designed as a piezoacoustic thin film resonator. A total layer thickness of the resonator consisting of electrode layers and zinc oxide film is, for example, 1 μm. By the little one
Filmdicke des Zinkoxidfilms beziehungsweise durch die kleine Gesamtschichtdicke ist die Masse des Resonators relativ niedrig. Dadurch erhöht sich die Resonanzfrequenz des Resonators. Durch die hohe Resonanzfrequenz ergibt sich eine hohe Massensensitivität gegenüber der Substanz. DieFilm thickness of the zinc oxide film or due to the small total layer thickness, the mass of the resonator is relatively low. This increases the resonance frequency of the resonator. The high resonance frequency results in a high mass sensitivity to the substance. The
Massensensitivität der Vorrichtung kann nach Gleichung (1) auf wenige Hz-pg_1-cm2 abgeschätzt werden. Beispielsweise beträgt die Massensensitivität bei einer Resonanzfrequenz von 1 GHz etwa 2,5 Hz-pg-1-cm2.Mass sensitivity of the device can be estimated according to equation (1) to a few Hz-pg _1 -cm 2 . For example, the mass sensitivity at a resonance frequency of 1 GHz is approximately 2.5 Hz-pg -1 cm 2 .
Das Fluid mit der Substanz kann ein Gas oder Gasgemisch sein. Insbesondere wird die Anordnung zur Detektion einer Substanz eines Fluid in Form einer Flüssigkeit verwendet. Wie bereits erwähnt, ist die Anordnung in der Form des BAW-Resonators i erster Linien zu DickenseherSchwingungen anregbar. Diese Dickenscherschwingungen erfahren im Gegensatz zu LängsSchwingungen nahezu keine Dämpfung durch eine Flüssigkeit, die direkt mit dem Resonator in Kontakt steht. Somit kann der Resonator auch in direktem Kontakt mit der Flüssigkeit eingesetzt werden.The fluid with the substance can be a gas or gas mixture. In particular, the arrangement is used for the detection of a substance of a fluid in the form of a liquid. As already mentioned, the arrangement in the form of the BAW resonator can be excited primarily to vibrate thick-sighted. In contrast to longitudinal vibrations, these thickness shear vibrations experience almost no damping due to a liquid that is in direct contact with the resonator. This means that the resonator can also be used in direct contact with the liquid.
Der Oberflächenabschnitt wird beispielsweise von einer chemisch sensitiven Beschichtung der Anordnung gebildet. Diese Beschichtung sorgt für die Sorption der Substanz . Die chemisch sensitive Beschichtung kann dabei auf einer oder auf beiden Elektroden der Anordnung bzw. des akustischen Resonators angeordnet sein. Die chemisch sensitive Beschichtung kann auch direkt auf dem Zinkoxidfilm aufgebracht sein.The surface section is formed, for example, by a chemically sensitive coating of the arrangement. This coating ensures the sorption of the substance. The chemically sensitive coating can be arranged on one or on both electrodes of the arrangement or the acoustic resonator. The chemically sensitive Coating can also be applied directly to the zinc oxide film.
Die Sorption umfasst sowohl eine Absorption als auch eine Adsorption. Bei der Absorption wird die Substanz beispielsweise durch eine Beschichtung des Resonators, die den Oberflächenabschnitt bildet, ohne Bildung einer Phasengrenze aufgenommen. Die Substanz wird in die Beschichtung inkorporiert . Bei der Adsorption kommt es hingegen zur Bildung einer Phasengrenze. Insbesondere denkbar ist dabei eine Adsorption in Form einer Physisorption. Die Substanz lagert sich am Oberflächenabschnitt des Resonators durch Van-der-Waals oder Dipol-Dipol-Wechselwirkungen an. Alternativ dazu kann auch eine Adsorption in Form einer Chemisorption stattfinden. Bei. einer Chemisorption lagert sich die Substanz am Oberflächenabschnitt unter Bildung einer chemischen Bindung an. Die chemische Bindung ist beispielsweise eine kovalente Bindung oder eine Wasserstoffbrückenbindung .Sorption includes both absorption and adsorption. During absorption, the substance is absorbed, for example, by a coating of the resonator, which forms the surface section, without forming a phase boundary. The substance is incorporated into the coating. In contrast, a phase boundary is formed during adsorption. Adsorption in the form of physisorption is particularly conceivable. The substance attaches to the surface section of the resonator through van der Waals or dipole-dipole interactions. Alternatively, adsorption in the form of chemisorption can also take place. In. chemisorption, the substance attaches to the surface section to form a chemical bond. The chemical bond is, for example, a covalent bond or a hydrogen bond.
Vorzugsweise findet die Sorption reversibel statt. Dies bedeutet, dass die Substanz vom Oberflächenabschnitt auch wieder desorbiert (entfernt) werden kann. Beispielsweise wird die Substanz durch Temperaturerhöhung des ■ Oberflächenabschnitts oder durch Einwirken eines reaktiven Stoffes wieder entfernt. Der reaktive Stoff ist beispielsweise eine Säure oder eine Lauge, mit deren Hilfe die bei der Chemisorption gebildeten Bindungen gelöst werden. Die Vorrichtung kann auf diese Weise mehrmals benutzt werden. Möglich ist auch, dass die Sorption irreversibel ist. Die Vorrichtung wird als Einwegsensor nur einmalig verwendet.Sorption preferably takes place reversibly. This means that the substance can also be desorbed (removed) from the surface section. For example, the substance is removed by increasing the temperature of the surface portion ■ or by exposure to a reactive substance. The reactive substance is, for example, an acid or an alkali, with the aid of which the bonds formed during chemisorption are released. The device can be used several times in this way. It is also possible that the sorption is irreversible. The device is used only once as a disposable sensor.
Als Substanz kommt jede denkbare chemische oder biologische Verbindung in Frage. So kann die Vorrichtung als Biosensor zur Detektion eines beliebigen Biomoleküls ausgestaltet sein. Das Biomolekül ist beispielsweise eine DNA (Deoxynucleic Acid) -Sequenz oder ein makromolekulares Protein. Der chemisch sensitive Oberflächenabschnitt bzw. die chemisch sensitive Beschichtung können aber auch zur Adsorption bestimmter gasförmiger Moleküle ausgestaltet sein. Derartige Moleküle sind beispielsweise Kohlenmonoxid, Kohlendioxid, Stickoxide oder Schwefeloxide. Niedermolekulare organische Gase wie Methan oder Ethan sind ebenfalls denkbarAny conceivable chemical or biological compound can be considered as a substance. The device can thus be designed as a biosensor for the detection of any biomolecule. The biomolecule is, for example, a DNA (deoxynucleic acid) sequence or a macromolecular protein. The chemical sensitive surface section or the chemically sensitive coating can also be designed for the adsorption of certain gaseous molecules. Such molecules are, for example, carbon monoxide, carbon dioxide, nitrogen oxides or sulfur oxides. Low molecular weight organic gases such as methane or ethane are also conceivable
Der Oberflächenabschnitt ist vorzugsweise derart ausgebildet, dass selektiv eine bestimmte Substanz oder Substanzklasse nach dem Schlüssellochprinzip sorbiert wird. Damit ist es möglich, aus einem Gemisch aus einer Vielzahl von Substanzen mit Hilfe der Anordnung selektiv eine bestimmte Substanz zu detektieren. Die Detektion umfasst dabei sowohl eine qualitative als auch quantitative Bestimmung der Substanz .The surface section is preferably designed such that a specific substance or class of substances is selectively sorbed according to the keyhole principle. It is thus possible to selectively detect a specific substance from a mixture of a large number of substances with the aid of the arrangement. The detection includes both a qualitative and quantitative determination of the substance.
In einer besonderen Ausgestaltung ist eine Vielzahl der beschriebenen Resonatoren zu einer Resonatormatrix zusammengefasst und jeder der Resonatoren bildet ein Matrixelement der Resonatormatrix. Dies bedeutet, dass jeder Resonator derart ausgelegt ist, dass er für eine bestimmte Substanz oder Substanzklasse sensitiv ist. Auf diese Weise können mit Hilfe der Anordnung Substanzge isehe qualitativ und/oder quantitativ analysiert werden. Bei einem Gassensor ist beispielsweise einer der Resonatoren sensitiv für Kohlenwasserstoffe, ein zweiter Resonator sensitiv für Schwefeloxide und ein weiterer Resonator sensitiv für Kohlenmonoxid. Bei einem Biosensor ist beispielsweise jeder der Resonatoren der einzelnen Matrixelemente gegenüber einer bestimmten DNA-Sequenz sensitiv. Somit lässt sich das Vorhandensein verschiedenen DNA-Sequenzen in einem Fluid parallel untersuchen.In a special embodiment, a large number of the resonators described are combined to form a resonator matrix and each of the resonators forms a matrix element of the resonator matrix. This means that each resonator is designed in such a way that it is sensitive to a specific substance or class of substances. In this way, the arrangement of substance can be analyzed qualitatively and / or quantitatively. In the case of a gas sensor, for example, one of the resonators is sensitive to hydrocarbons, a second resonator is sensitive to sulfur oxides and another resonator is sensitive to carbon monoxide. In the case of a biosensor, for example, each of the resonators of the individual matrix elements is sensitive to a specific DNA sequence. The presence of different DNA sequences in a fluid can thus be examined in parallel.
Der Resonator kann auf einem beliebigen Substrat angeordnet sein. Vorzugsweise zeichnet sich das Substrat durch ein Material mit einem geringen Verlust für Hochfrequenzsignale aus. Ein derartiges Material ist beispielsweise Saphir. In einer bevorzugten Ausgestaltung ist der Zinkoxidfilm auf einem Substrat aus einem Halbleitermaterial angeordnet. Vorzugsweise ist das Halbleitermaterial aus der Gruppe Silizium und/oder Galliumarsenid ausgewählt. Das Substrat kann dabei einkristallin oder polykristallin sein. Die genannten Halbleitermaterialien eignen sich zur Anwendung von Bipolar- und CMOS (Complementary Metal Oxide Semiconductor) - Technologie zur Integration von Ansteuerungs- und/oder Auswerteeinrichtungen des Resonators .The resonator can be arranged on any substrate. The substrate is preferably characterized by a material with a low loss for high-frequency signals. Such a material is, for example, sapphire. In a preferred embodiment, the zinc oxide film is arranged on a substrate made of a semiconductor material. The semiconductor material is preferably selected from the group consisting of silicon and / or gallium arsenide. The substrate can be single crystal or polycrystalline. The semiconductor materials mentioned are suitable for the use of bipolar and CMOS (Complementary Metal Oxide Semiconductor) technology for integrating control and / or evaluation devices of the resonator.
Vorzugsweise weist die Anordnung mindestens eine Einrichtung zur akustischen Isolation des Resonators und des Substrats auf . Der Resonator und das Substrat sind akustische voneinander isoliert. Durch die akustische Isolation ist gewährleistet, dass die Resonanzfrequenz des Resonators unabhängig vom Substrat ist . Es resultiert eine relativ hohe Massensensitivität. Die Einrichtung zur akustischen Isolation ist beispielsweise ein Bragg-Reflektor, der aus λ/4-dicken Schichten unterschiedlicher akustischer Impedanz besteht. Alternativ dazu wird die Einrichtung durch einen Hohlraum im Substrat gebildet.The arrangement preferably has at least one device for acoustically isolating the resonator and the substrate. The resonator and the substrate are acoustically isolated from each other. The acoustic insulation ensures that the resonance frequency of the resonator is independent of the substrate. The result is a relatively high mass sensitivity. The device for acoustic isolation is, for example, a Bragg reflector, which consists of λ / 4 thick layers of different acoustic impedance. Alternatively, the device is formed by a cavity in the substrate.
Zusammenfassen ergeben sich mit der Erfindung folgende wesentlichen Vorteile:To summarize, the following significant advantages result with the invention:
• Auf der Basis der vorliegenden Erfindung ist ein biaxial texturierter, polykristalliner Zinkoxidfilm auf einem beliebigen Substrat zugänglich.• Based on the present invention, a biaxially textured, polycrystalline zinc oxide film is accessible on any substrate.
• Der Zinkoxidfilm ist dabei homogen. Dies bedeutet, dass der gesamte Film in Dickenrichtung als auch entlang einer lateralen Ausdehnung biaxial texturiert werden kann.• The zinc oxide film is homogeneous. This means that the entire film can be biaxially textured in the thickness direction as well as along a lateral dimension.
• Die Zinkoxid-Einkristalle sind bevorzugt derart orientiert, dass der Zinkoxidfilm als Bestandteil eines BAW-Resonators im Wesentlichen nur zu Dickenscherschwingungen angeregt werden kann. Der BAW- Resonator kann ohne starke Dämpfung seiner• The zinc oxide single crystals are preferably oriented in such a way that the zinc oxide film as part of a BAW resonator can essentially only be excited to vibrate in thickness. The BAW Resonator can be without strong damping
Resonanzfrequenz in direktem Kontakt mit einer Flüssigkeit eingesetzt werden.Resonance frequency can be used in direct contact with a liquid.
• Die Anordnung kann zur Detektion einer Substanz ausgestaltet sein. Die Anordnung zeichnet sich dabei durch eine hohe Massensensitivität aus.• The arrangement can be designed for the detection of a substance. The arrangement is characterized by a high mass sensitivity.
Anhand mehrerer Ausführungsbeispiele und der dazugehörigen Figuren wird die Erfindung im Folgenden näher erläutert. Die Figuren sind schematisch und stellen keine maßstabsgetreuen Abbildungen dar.The invention is explained in more detail below with the aid of several exemplary embodiments and the associated figures. The figures are schematic and do not represent true-to-scale illustrations.
Figur la zeigt eine Anordnung aus einem Zinkoxidfilm auf einer Substratoberfläche eines Substrats imFigure la shows an arrangement of a zinc oxide film on a substrate surface of a substrate in
Querschnitt von der Seite.Cross section from the side.
Figur lb zeigt die Anordnung in Aufsicht auf den Zinkoxidfilm.Figure lb shows the arrangement in plan view of the zinc oxide film.
Figur 2 zeigt eine Anordnung in Form eines Biosensors.Figure 2 shows an arrangement in the form of a biosensor.
Figur 3 zeigt eine Anordnung mit mehreren Biosensoren im Querschnitt.Figure 3 shows an arrangement with several biosensors in cross section.
Figur 4 zeigt ein Verfahren zum Detektieren einer SubstanzFIG. 4 shows a method for detecting a substance
Figur 5 zeigt ein Verfahren zum Herstellen des Zinkoxid Films.FIG. 5 shows a method for producing the zinc oxide film.
Die Anordnung 1 besteht aus einem polykristallinen Zinkoxidfilm 2 auf einem Substrat 3 aus Silizium (Figuren la und lb) . Der Zinkoxidfilm 2 ist auf einer Substratoberfläche 4 des Substrats 3 aufgebracht. Der Zinkoxidfilm 2 besteht aus einer Vielzahl von Zinkoxid-Einkristallen. Die [100]-The arrangement 1 consists of a polycrystalline zinc oxide film 2 on a substrate 3 made of silicon (Figures la and lb). The zinc oxide film 2 is applied to a substrate surface 4 of the substrate 3. The zinc oxide film 2 consists of a large number of zinc oxide single crystals. The [100] -
Gittergeraden der einzelnen Zinkoxid-Einkristalle weisen eine Ausrichtung 6 in Richtung der Flächennormalen 5 der Substratoberfläche 4 auf. Die [001] -Gittergeraden der Zinkoxid-Einkristalle sind zueinander parallel und entlang der Substratoberfläche 4 ausgerichtet. Die [001]- Gittergeraden weisen eine Ausrichtung 7 senkrecht zur Flächennormalen 5 auf. In dieser Konstellation ist der Zinkoxidfilm 2 zu Dickenscherschwingungen 12 entlang der lateralen Ausdehnung 17 des Zinkoxidfilms 2 anregbar.Grid lines of the individual zinc oxide single crystals have an orientation 6 in the direction of the surface normal 5 of the Substrate surface 4. The grating lines of the zinc oxide single crystals are parallel to one another and aligned along the substrate surface 4. [001] The grid lines have an orientation 7 perpendicular to the surface normal 5. In this constellation, the zinc oxide film 2 can be excited to give thickness shear vibrations 12 along the lateral extent 17 of the zinc oxide film 2.
Zum Herstellen des Zinkoxidfilms 2 auf dem Substrat 3 wird das IBAD-Verfahren benutzt (Figur 5) . Dabei wird in einerThe IBAD method is used to produce the zinc oxide film 2 on the substrate 3 (FIG. 5). It is in one
Sputterkammer 101 das Zinkoxid auf der Substratoberfläche 4 des Substrats 3 abgeschieden. Die Sputterkammer 101 weist eine Sauerstoffatmosphäre auf. Zum Abscheiden wird Zinkoxid von einem Sputtertarget 102 aus Zinkoxid durch Sputterionen 103 abgesputtert (verdampft) . Die Sputterionen sindSputter chamber 101 deposited the zinc oxide on the substrate surface 4 of the substrate 3. The sputtering chamber 101 has an oxygen atmosphere. For deposition, zinc oxide is sputtered (evaporated) from a sputtering target 102 made of zinc oxide by sputtering ions 103. The sputterions are
Argonionen mit einer Energie zwischen 500 eV und 1500 eV. Diese Argonionen werden von einer Ionenquelle 106 erzeugt und auf das Sputtertarget 102 gelenkt. Die Sputterionen 103 treffen schräg auf das Sputtertarget 102 auf und lösen dort von der Oberfläche des Sputtertargets 102 Zinkoxid-Teilchen 107 heraus. Diese Zinkoxid-Teilchen 107 gelangen an das gegenüber den Sputtertarget 102 angeordnete Substrat 3 und werden dort an der Substratoberfläche 4 des Substrats 3 abgeschieden .Argon ions with an energy between 500 eV and 1500 eV. These argon ions are generated by an ion source 106 and directed onto the sputtering target 102. The sputtering ions 103 strike the sputtering target 102 at an angle and release zinc oxide particles 107 there from the surface of the sputtering target 102. These zinc oxide particles 107 reach the substrate 3 arranged opposite the sputtering target 102 and are deposited there on the substrate surface 4 of the substrate 3.
Während des Abscheidens des Zinkoxids wird ein assistierender Strahl von Ionen 104 schräg auf die Substratoberfläche 4 des Substrats 3 unter einem vorbestimmten Einfallswinkel 105 bezüglich der Flächennormalen 5 der Substratoberfläche 4 gerichtet. Der Einfallswinkel beträgt 58°. Die Ionen 104 sind Argonionen mit einer Energie von etwa 350 eV. Diese Argonionen werden von einer weiteren Ionenquelle 108 erzeugt und auf die Substratoberfläche 4 gerichtet.During the deposition of the zinc oxide, an assisting beam of ions 104 is directed obliquely onto the substrate surface 4 of the substrate 3 at a predetermined angle of incidence 105 with respect to the surface normal 5 of the substrate surface 4. The angle of incidence is 58 °. The ions 104 are argon ions with an energy of approximately 350 eV. These argon ions are generated by a further ion source 108 and directed onto the substrate surface 4.
Die Anordnung 1 wird zur Detektion einer Substanz verwendet. Dazu ist die Anordnung 1 zu einem piezoakustischen Resonator (BAW-Resonator) 10 ausgestaltet, der auf einem Halbleitersubstrat 3 aus Silizium aufgebracht ist (Figur 2) . Der Resonator 10 weist den piezoelektrisch aktiven Zinkoxidfilm 2 auf. Die Filmdicke 11 des Zinkoxidfilms beträgt ca. 0,8 μm. Die laterale Ausdehnung 17 des Resonators 10 beträgt ca. 100 μm.The arrangement 1 is used for the detection of a substance. For this purpose, the arrangement 1 is configured as a piezoacoustic resonator (BAW resonator) 10 which is based on a Semiconductor substrate 3 made of silicon is applied (Figure 2). The resonator 10 has the piezoelectrically active zinc oxide film 2. The film thickness 11 of the zinc oxide film is approximately 0.8 μm. The lateral extent 17 of the resonator 10 is approximately 100 μm.
Die Elektroden 8 und 9 sind in Form von Elektrodenschichten an zwei voneinander abgekehrten Seiten des Zinkoxidfilms 2 angeordnet. Die Schichtdicke der Elektrodenschichten 8 und 9 beträgt jeweils ca. 0,1 μm. Die Elektroden 8 und 9 sind ausThe electrodes 8 and 9 are arranged in the form of electrode layers on two sides of the zinc oxide film 2 facing away from one another. The layer thickness of the electrode layers 8 and 9 is in each case approximately 0.1 μm. The electrodes 8 and 9 are off
Gold. Eine elektrische Isolierung 18 aus Aluminiumoxid trennt die Elektroden 8 und 9 zusätzlich. Durch elektrische Ansteuerung der Elektroden 8 und 9 wird der Resonator 10 zu den Dickenscherschwingungen 12 angeregt .Gold. An electrical insulation 18 made of aluminum oxide additionally separates the electrodes 8 and 9. The resonator 10 is excited to the thickness shear vibrations 12 by electrical control of the electrodes 8 and 9.
Der Resonator 10 verfügt über einen Oberflächenabschnitt 13, an dem eine Substanz eines Fluids 15 sorbiert werden kann. Dazu verfügt der Resonator 10 über eine chemisch sensitive Beschichtung 14. Die chemisch sensitive Beschichtung 14 ist auf der Elektrode 8 angebracht.The resonator 10 has a surface section 13 on which a substance of a fluid 15 can be sorbed. For this purpose, the resonator 10 has a chemically sensitive coating 14. The chemically sensitive coating 14 is applied to the electrode 8.
Um die Massensensitivität des Resonators 10 für eine bestimmte Substanz zu erhöhen, werden das Halbleitersubstrat 3 und der Resonator 10 mit Hilfe einer Einrichtung zur akustischen Isolation 16 akustisch voneinander isoliert.In order to increase the mass sensitivity of the resonator 10 for a specific substance, the semiconductor substrate 3 and the resonator 10 are acoustically isolated from one another with the aid of a device for acoustic isolation 16.
Gemäß dem vorliegenden Beispiel ist die Einrichtung 16 ein Bragg-Reflektor mit λ/4-dicken Schichten unterschiedlicher Impedanz .According to the present example, the device 16 is a Bragg reflector with λ / 4 thick layers of different impedance.
Figur 3 zeigt eine Vorrichtung 1 mit drei Resonatoren 10 im einem seitlichen Querschnitt. Die Resonatoren 10 sind auf einem Halbleitersubstrat 3 aus Silizium zu einer Resonatormatrix 19 aufgebracht. Die Resonatoren 10 bilden je ein Matrixelement 20 der Resonatormatrix 19. Jeder der Resonatoren 10 weist eine laterale Ausdehnung 17 von etwa 100 μm auf. Ein Abstand 21 zwischen benachbarten Matrixelementen 20 beträgt 100 μm. Jedes der Matrixelemente 21 verfügt über einen für eine bestimmte Substanz sensitiven Resonator 10. Es liegt eine Vorrichtung zur Detektion einer Vielzahl von Substanzen eines Fluids 15 vor.FIG. 3 shows a device 1 with three resonators 10 in a lateral cross section. The resonators 10 are applied to a semiconductor substrate 3 made of silicon to form a resonator matrix 19. The resonators 10 each form a matrix element 20 of the resonator matrix 19. Each of the resonators 10 has a lateral dimension 17 of approximately 100 μm. A distance 21 between adjacent matrix elements 20 is 100 μm. Each of the matrix elements 21 has a resonator 10 sensitive to a specific substance. There is a device for detecting a large number of substances in a fluid 15.
Die Anordnung wird zur Detektion einer Substanz eines Fluids 15 in Form einer Flüssigkeit verwendet. Zur Detektion der Substanz des Fluids 15 werden jeweils in einem ersten Schritt der chemisch sensitive Oberflächenabschnitt 13 des Resonators 10 und das Fluid 15 zusammengebracht (Figur 4, Schritt 41) . Das Fluid 15 und der Resonator 10 werden derart zusammengebracht, dass die Substanz des Fluids 15 auf den jeweiligen Oberflächenabschnitten 13 des Resonators 10 sorbiert werden kann. Durch die Sorption ändert sich die Masse des Resonators 10. Durch nachfolgende Messung der Resonanzfrequenzen des Resonators 10 (Figur 4, Schritt 42) kann auf die Art der Substanz und deren Konzentration im Fluid 15 geschlossen werden. Durch die Sorption der Substanz verändert sich die Resonanzfrequenz des Resonators 10 im Vergleich zur Resonanzfrequenz des Resonators 10, an dessen Oberflächenabschnitt 13 keine Substanz sorbiert ist. Um die Änderung der Resonanzfrequenz bestimmen zu können, wird ein Resonator 10 mit bekannter Resonanzfrequenz verwendet. In einer alternativen Ausführung wird vor dem Zusammenbringen des Fluids und des Resonators die Resonanzfrequenz des Resonators ohne sorbierte Substanz bestimmt. The arrangement is used for the detection of a substance of a fluid 15 in the form of a liquid. To detect the substance of the fluid 15, the chemically sensitive surface section 13 of the resonator 10 and the fluid 15 are brought together in a first step (FIG. 4, step 41). The fluid 15 and the resonator 10 are brought together in such a way that the substance of the fluid 15 can be sorbed on the respective surface sections 13 of the resonator 10. The mass of the resonator 10 changes as a result of the sorption. The type of substance and its concentration in the fluid 15 can be inferred from subsequent measurement of the resonance frequencies of the resonator 10 (FIG. 4, step 42). The sorption of the substance changes the resonance frequency of the resonator 10 compared to the resonance frequency of the resonator 10, on the surface section 13 of which no substance is sorbed. In order to be able to determine the change in the resonance frequency, a resonator 10 with a known resonance frequency is used. In an alternative embodiment, the resonance frequency of the resonator without the sorbed substance is determined before the fluid and the resonator are brought together.

Claims

Patentansprüche claims
1. Anordnung (1) aus einem Zinkoxidfilm (2) auf einer Substratoberfläche (4) eines Substrats (3), aufweisend - eine Vielzahl von Zinkoxid-Einkristallen mit jeweils einer [100] -Gittergeraden, die im Wesentlichen parallel zu einer Flächennormalen der Substratoberfläche ausgerichtet ist, dadurch gekennzeichnet, dass - die Zinkoxid-Einkristalle [001] -Gittergeraden aufweisen, die im Wesentlichen zueinander parallel ausgerichtet sind.1. Arrangement (1) of a zinc oxide film (2) on a substrate surface (4) of a substrate (3), comprising - a multiplicity of zinc oxide single crystals, each with a [100] grating straight line, which is essentially parallel to a surface normal of the substrate surface is aligned, characterized in that - the zinc oxide single crystals have [001] lattice lines which are aligned essentially parallel to one another.
2. Anordnung nach Anspruch 1, mit - mindestens einer am Zinkoxidfilm (2) angeordneten2. Arrangement according to claim 1, with - at least one on the zinc oxide film (2) arranged
Elektrode (8, 9) und mindestens einer am Zinkoxidfilm (2) angeordneten weiteren Elektrode (9, 8) , wobei der Zinkoxidfilm (2) und die Elektroden (8, 9) derart zu einem piezoakustischen Resonator (10) angeordnet sind, dass eine elektrische Ansteuerung der Elektroden (8, 9) zu einer piezoakustischen Schwingung (12) des ResonatorsElectrode (8, 9) and at least one further electrode (9, 8) arranged on the zinc oxide film (2), the zinc oxide film (2) and the electrodes (8, 9) being arranged to form a piezoacoustic resonator (10) such that a electrical control of the electrodes (8, 9) to a piezoacoustic oscillation (12) of the resonator
(10) mit einer bestimmten Resonanzfrequenz führt.(10) leads with a certain resonance frequency.
3. Anordnung nach Anspruch 1 oder 2, wobei eine Filmdicke (11) des Zinkoxidfilms (2) aus dem Bereich von einschließlich 0,1 μm bis einschließlich 20 μm und die Resonanzfrequenz der piezoakustischen Schwingung (12) des Resonators (10) aus dem Bereich von einschließlich 500 MHz bis einschließlich 10 GHz ausgewählt ist.3. Arrangement according to claim 1 or 2, wherein a film thickness (11) of the zinc oxide film (2) from the range of 0.1 microns up to and including 20 microns and the resonance frequency of the piezoacoustic oscillation (12) of the resonator (10) from the range from 500 MHz up to and including 10 GHz is selected.
4. Anordnung nach Anspruch 2 oder 3, mit - einem gegenüber einer Substanz eines Fluids (15) chemisch sensitiven Oberflächenabschnitt (13) zur Sorption der Substanz, wobei die Resonanzfrequenz des Schwingung (12) des Resonators (10) abhängig ist von einer Menge der Substanz, die auf dem chemisch sensitiven Oberflächenabschnitt (13) sorbiert ist.4. Arrangement according to claim 2 or 3, with - a surface portion (13) chemically sensitive to a substance of a fluid (15) for sorption of the substance, wherein the resonance frequency of the oscillation (12) of the resonator (10) depends on an amount of the substance that is sorbed on the chemically sensitive surface section (13).
5. Anordnung nach einem der Ansprüche 1 bis 4, wobei das Substrat (3) ein Halbleitermaterial aufweist.5. Arrangement according to one of claims 1 to 4, wherein the substrate (3) comprises a semiconductor material.
6. Anordnung nach einem der Ansprüche 2 bis 5, wobei mindestens eine Einrichtung (16) zur akustischen6. Arrangement according to one of claims 2 to 5, wherein at least one device (16) for acoustic
Isolation des Resonators (19) und des Substrats (3) vorhanden ist.Isolation of the resonator (19) and the substrate (3) is present.
7. Anordnung nach einem der Ansprüche 2 bis 6, wobei der chemisch sensitive Oberflächenabschnitt (13) zur7. Arrangement according to one of claims 2 to 6, wherein the chemically sensitive surface section (13) for
Sorption der Substanz des Fluids (15) von einer gegenüber der Substanz chemisch sensitiven Beschichtung (14) des Resonators (10) gebildet ist.Sorption of the substance of the fluid (15) is formed by a coating (14) of the resonator (10) that is chemically sensitive to the substance.
8. Verfahren zum Herstellen einer Anordnung eines Zink- Oxid-Films auf einer Substratoberfläche (4) eines Substrats (3) nach einem der Ansprüche 1 bis 7, durch Abscheiden von Zinkoxid auf der Substratoberfläche, wobei zum Abscheiden ein Abtragen von Zinkoxid und/oder einer Vorstufe des Zinkoxids von einer Quelle des Zinkoxids und/oder der Vorstufe des Zinkoxids durchgeführt wird und während des Abscheidens ein Strahl von Ionen schräg auf die Substratoberfläche des Substrats unter einem vorbestimmten Einfallswinkel bezüglich der Flächennormalen der Substratoberfläche gerichtet wird.8. A method for producing an arrangement of a zinc oxide film on a substrate surface (4) of a substrate (3) according to any one of claims 1 to 7, by depositing zinc oxide on the substrate surface, wherein for deposition a removal of zinc oxide and / or a precursor of the zinc oxide is carried out from a source of the zinc oxide and / or the precursor of the zinc oxide and during the deposition a beam of ions is directed obliquely onto the substrate surface of the substrate at a predetermined angle of incidence with respect to the surface normal of the substrate surface.
9. Verfahren nach Anspruch 8, wobei als Quelle des9. The method according to claim 8, wherein as the source of
Zinkoxids und/oder der Vorstufe des Zinkoxids ein Sputtertarget verwendet wird und zum Abtragen einZinc oxide and / or the precursor of the zinc oxide a sputtering target is used and for removal
Absputtern des Zinkoxid und/oder der Vorstufe des Zinkoxids von dem Sputtertarget durch Sputterionen durchgeführt wird.Sputtering of the zinc oxide and / or the precursor of Zinc oxide is carried out from the sputtering target by sputtering ions.
10. Verfahren nach Anspruch 9, wobei der Einfallswinkel aus dem Bereich von einschließlich 30° bis einschließlich10. The method of claim 9, wherein the angle of incidence is in the range of 30 ° up to and including
70° ausgewählt wird.70 ° is selected.
11. Verwendung der Anordnung nach einem der Ansprüche 2 bis 10 zur Detektion einer Substanz eines Fluids (15) mit den Schritten: a) Zusammenbringen des Fluids (15) und der Anordnung (1) derart, dass die Substanz am chemisch sensitiven Oberflächenabschnitt (13) des Resonators (10) sorbiert werden kann und b) Bestimmen einer Resonanzfrequenz des Resonators (10) , wobei aus der Resonanzfrequenz auf die am chemisch sensitiven Oberflächenabschnitt (13) sorbierte Menge • der Substanz geschlossen wird.11. Use of the arrangement according to one of claims 2 to 10 for the detection of a substance of a fluid (15) with the steps: a) bringing together the fluid (15) and the arrangement (1) such that the substance on the chemically sensitive surface portion (13 can be sorbed) of the resonator (10) and b) determining a resonant frequency of the resonator (10), (13) • sorbed amount of the substance concluded from the resonance frequency to the most chemically sensitive surface portion.
12. Verwendung nach Anspruch 11, wobei als Fluid (15) eine Flüssigkeit verwendet wird. 12. Use according to claim 11, wherein a liquid is used as the fluid (15).
PCT/EP2003/014342 2003-01-30 2003-12-16 Arrangement consisting of a zinc oxide film applied to a substrate, method for producing said arrangement, and use of the same WO2004067797A1 (en)

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DE102006003847A1 (en) * 2006-01-26 2007-08-09 Siemens Ag Method and apparatus for producing a polycrystalline ceramic film on a substrate, capacitor structure with the ceramic film and use of the capacitor structure
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WO2007085549A2 (en) * 2006-01-26 2007-08-02 Siemens Aktiengesellschaft Method and device for the production of a polycrystalline ceramic film on a substrate capacitive structure comprising said ceramic film and use of said capacitive structure
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CN104379795A (en) * 2012-06-29 2015-02-25 西门子公司 Method for producing a polycrystalline ceramic film
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US10553780B2 (en) 2012-06-29 2020-02-04 Siemens Aktiengesellschaft Method for producing a polycrystalline ceramic film
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