WO2002042527A1 - Substrat de diamant possedant un film mince piezo-electrique et procede de fabrication de celui-ci - Google Patents
Substrat de diamant possedant un film mince piezo-electrique et procede de fabrication de celui-ci Download PDFInfo
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- WO2002042527A1 WO2002042527A1 PCT/JP2001/010106 JP0110106W WO0242527A1 WO 2002042527 A1 WO2002042527 A1 WO 2002042527A1 JP 0110106 W JP0110106 W JP 0110106W WO 0242527 A1 WO0242527 A1 WO 0242527A1
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- thin film
- diamond substrate
- piezoelectric thin
- polycrystalline diamond
- diamond
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- 239000010432 diamond Substances 0.000 title claims abstract description 219
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 218
- 239000000758 substrate Substances 0.000 title claims abstract description 168
- 239000010409 thin film Substances 0.000 title claims abstract description 153
- 238000000034 method Methods 0.000 title claims abstract description 42
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- 238000000608 laser ablation Methods 0.000 claims description 38
- 239000000203 mixture Substances 0.000 claims description 37
- 239000002994 raw material Substances 0.000 claims description 35
- 238000002441 X-ray diffraction Methods 0.000 claims description 31
- 239000012808 vapor phase Substances 0.000 claims description 21
- 239000012071 phase Substances 0.000 claims description 15
- 230000015572 biosynthetic process Effects 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 8
- 238000003786 synthesis reaction Methods 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 238000010897 surface acoustic wave method Methods 0.000 abstract description 12
- 239000000463 material Substances 0.000 abstract description 11
- 230000003287 optical effect Effects 0.000 abstract description 6
- 230000005684 electric field Effects 0.000 description 22
- 230000010287 polarization Effects 0.000 description 17
- 239000013078 crystal Substances 0.000 description 16
- 239000010408 film Substances 0.000 description 14
- 230000003746 surface roughness Effects 0.000 description 9
- 230000005540 biological transmission Effects 0.000 description 8
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 7
- 229910001882 dioxygen Inorganic materials 0.000 description 7
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 238000002003 electron diffraction Methods 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 238000001308 synthesis method Methods 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 5
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- 238000004993 emission spectroscopy Methods 0.000 description 5
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- 230000035484 reaction time Effects 0.000 description 5
- 238000000151 deposition Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 229910052594 sapphire Inorganic materials 0.000 description 4
- 239000010980 sapphire Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000011109 contamination Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
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- 230000001678 irradiating effect Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 241000652704 Balta Species 0.000 description 1
- 241000828585 Gari Species 0.000 description 1
- 229910018068 Li 2 O Inorganic materials 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
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- 241000018646 Pinus brutia Species 0.000 description 1
- 239000006061 abrasive grain Substances 0.000 description 1
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- 238000001914 filtration Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
-
- 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
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
- C23C14/325—Electric arc evaporation
-
- H—ELECTRICITY
- H03—ELECTRONIC CIRCUITRY
- H03H—IMPEDANCE NETWORKS, e.g. RESONANT CIRCUITS; RESONATORS
- H03H3/00—Apparatus or processes specially adapted for the manufacture of impedance networks, resonating circuits, resonators
- H03H3/007—Apparatus or processes specially adapted for the manufacture of impedance networks, resonating circuits, resonators for the manufacture of electromechanical resonators or networks
- H03H3/08—Apparatus or processes specially adapted for the manufacture of impedance networks, resonating circuits, resonators for the manufacture of electromechanical resonators or networks for the manufacture of resonators or networks using surface acoustic waves
-
- H—ELECTRICITY
- H03—ELECTRONIC CIRCUITRY
- H03H—IMPEDANCE NETWORKS, e.g. RESONANT CIRCUITS; RESONATORS
- H03H9/00—Networks comprising electromechanical or electro-acoustic devices; Electromechanical resonators
- H03H9/02—Details
- H03H9/02535—Details of surface acoustic wave devices
- H03H9/02543—Characteristics of substrate, e.g. cutting angles
- H03H9/02582—Characteristics of substrate, e.g. cutting angles of diamond substrates
-
- 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
-
- 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
- H10N30/704—Piezoelectric or electrostrictive devices based on piezoelectric or electrostrictive films or coatings
- H10N30/706—Piezoelectric or electrostrictive devices based on piezoelectric or electrostrictive films or coatings characterised by the underlying bases, e.g. substrates
-
- 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
- H10N30/80—Constructional details
- H10N30/85—Piezoelectric or electrostrictive active materials
- H10N30/853—Ceramic compositions
- H10N30/8542—Alkali metal based oxides, e.g. lithium, sodium or potassium niobates
Definitions
- the present invention relates to a diamond substrate having a piezoelectric thin film formed thereon and a method of manufacturing the same.
- the present invention relates to a diamond substrate having a piezoelectric thin film used for a surface acoustic wave element and an optical element material that can be used in a high frequency band, and a method for manufacturing the same.
- SAW surface acoustic wave devices that use surface acoustic waves (hereinafter abbreviated as SAW) propagating on the surface of solids have various features such as small size, light weight, high temperature stability, and excellent phase characteristics. are doing.
- SAW surface acoustic wave devices that can be used in high-frequency bands
- materials that have a high speed of propagation of surface acoustic waves are used.
- narrowing the electrode pitch depends on the semiconductor device manufacturing technology and has its limitations.
- diamond is the fastest material with a high surface acoustic wave propagation speed. Therefore, a laminated structure in which three LiNb ⁇ layers are arranged on diamond has been proposed as disclosed in Japanese Patent Application Laid-Open No. 7-321596. According to this document, diamond (1 1 1) L i Nb 0 3 c-axis oriented on the surface is formed by an RF magnetron sputtering method, sigma values representing the c-axis orientation is 5 or less (more Is 4 or less), and the c-axis orientation is not so good. Japanese Patent Application Laid-Open No.
- 5-78200 discloses a method for synthesizing a Li (Nb x Ta x — x ) 0 3 (0 ⁇ x ⁇ 1) thin film on a sapphire substrate. This document discloses that a single-phase L i (Nb x T a! _ X ) O 3 (0 ⁇ x ⁇ 1) thin film can be obtained, but there is no disclosure about the quality of the formed thin film. . Further, Japanese Patent Laid-Open No. 5- 319993, L i Nb 0 3 layer formed surface acoustic wave device has been proposed on sapphire. Although the orientation of the three layers of LiNb03 is good, sapphire has a better sound than diamond.
- L i Nb 0 3 single crystal or L i T a 0 3 single crystal is industrially by Chi Yokurarusuki method (CZ method) has been grown.
- the congruent composition is selected so that the melt and composition do not change as the solidification of the crystal progresses.
- 0 is the stoichiometric composition ing.
- the ratio of Li to Nb affects the properties of Li NbO 3 single crystal.
- the ratio of Li to Nb x Ta x _ x is also important in the above-mentioned Li (N b x T a ⁇ _ x ) 0 3 (0 ⁇ x ⁇ 1) thin film, and good piezoelectric properties and electrochemical to bring out the characteristics and nonlinear-optic properties, atomic composition ratio L i / N b x T a ! It is necessary to control the value of _ x (hereinafter also simply referred to as the ratio Li / Nb x T ai _ x ) to 0.80 or more and 1.10 or less.
- the raw material target Is known to make the Li composition excessive.
- Japanese Patent Laid-Open No. 5- 78200 when forming a L i Nb0 3 thin film on a sapphire substrate, that have been devised to be in the L IZNb ratio of target 1.5 or 3.5 or less. And power, and, to form a L i Nb0 3 on the diamond substrate in this way, at the substrate temperature is below 1000 ° C was discovered that L IZNb ratio of the thin film is 1.10 or more.
- L i (Nb x T a - x) 0 3 when the polarization region there are multiple, cancel differ between regions of ⁇ Jo number, the entire not have the piezoelectric characteristics, on the die Yamondo L i (Nb x T a! _ X ) 0 3 A polarization treatment needs to be performed when or after the thin film is formed.
- L i (Nb x T a ! _ X) 0 3 is, polarization processing after crystallization is known to be difficult.
- the ferroelectric material can be made uniform in polarization by heating it above the Curie temperature and then applying an electric field higher than the coercive electric field to the crystal.
- the composite substrate of the polycrystalline diamond is L i Nb0 3 thin film as an insulator, avalanche current generated Then charge is concentrated on the interface between the L i Nb 0 3 thin film and the diamond, polarization treatment is good efficiency In addition, dielectric breakdown occurs. Therefore, in the composite substrate formed with L i NbO 3 thin film on a diamond substrate, it is desirable to perform the polarization treatment at the same time for forming a film which forms a L i Nb0 3 thin film.
- L i (Nb x T a ! _ X) to form 0 but 3 to improve the c-axis orientation of the thin film was made from a conventional, thin film was also formed by well-c-axis alignment
- the piezoelectric properties are not always good.
- the L i (Nb x T a J — x ) O 3 thin film has polarization along the c-axis direction.
- + Z— of the polarization direction may be mixed depending on the region. In such a case, there is no piezoelectric characteristic in the entire thin film where the piezoelectric characteristic is locally exhibited, and the characteristic of the element cannot be obtained. Disclosure of the invention
- the present invention has been devised to overcome the above problems. That is, the present invention provides a diamond substrate on which a thin film of Li (Nb x Ta! _ X ) 0 3 (0 ⁇ x ⁇ 1) which is C-axis oriented and has good piezoelectric properties and a method of manufacturing the same are provided. is there.
- the present invention uses a laser ablation method in which a pulsed laser beam is condensed and vaporized instantaneously on a raw material target, and a piezoelectric thin film L i (Nb x T a ⁇ _ x ) 0 3 (where O ⁇ x ⁇ l) be formed on the thin film (1 10) oriented polycrystalline diamond substrate on, c-axis oriented, form a favorable L i (Nb x T a! _ x) 0 3 thin film of piezoelectric characteristics It has been found that a diamond substrate can be obtained.
- ⁇ (i.) Is 15% or more. More preferably, it is at least 40%. In addition, when it is not oriented, the ratio ⁇ (!! 0) is less than 15%.
- the outermost surface of the polycrystalline diamond is covered with an amorphous layer having a thickness of 1 nm or more and 50 nm or less.
- Such polycrystalline diamond, single THE on a substrate one Abureshiyon method
- the formed L i (Nb x T a! _ X) 0 3 thin film, c-axis orientation is good piezoelectric properties are also good.
- the c-axis orientation is defined as follows.
- the gamma c is at 50% or more, the value is larger desirable.
- the laser used in the laser ablation method is not particularly limited, but it is preferable to use a laser having a wavelength of 360 nm or less and a pulse width of 1 ⁇ sec or less. Such lasers, there are etc.
- a r F and F a 2 excimer laser, in particular, K r F excimer laser with a wavelength of 24 8 nm is preferable.
- the laser light density is preferably 1 J / cm 2 or more, and the laser frequency is preferably about 1 to 50 Hz.
- the temperature of the polycrystalline diamond substrate at the time of laser ablation may be 400 ° C. or higher, but is preferably 10000 ° C. or lower since the polycrystalline diamond is degraded at 100 ° C. or higher. .
- the atmosphere is oxygen, ozone, N 2 0, N0 acid I arsenide atmosphere is preferably made of 2, atmospheric pressure is preferably in the range of 0. 1 ⁇ 1 0 0 P a. Further, the distance between the piezoelectric thin film raw material target and the polycrystalline diamond substrate is preferably in the range of 10 to 100 Omm.
- the atomic composition ratio between Li and Nb x T a ⁇ _ x of the formed L i (N b x T a! _ X ) 0 3 thin film ranges from 0.80 to 1.10
- the temperature of the polycrystalline diamond substrate and the atomic composition ratio of Li and Nb x T ai x of the piezoelectric thin film material target, Li ZN b x T a _ x are plotted using orthogonal coordinate axes. Point A in Fig.
- composition ratio 0.9 same display after substrate temperature 400 ° C
- B 0.9, 1000 ° C
- C 2.5, 10000 ° C
- D 2.5, 700 ° C
- E 1.5, 400 ° C
- Crystalline, and the orientation of the good L i (N b x T a x _ x) O 3 thin film does not include the phase such as amorphous not crystallized, L i (N b x T a! _ X) 0 3 A film in which the (01) plane of the thin film is parallel to the substrate (so-called c-axis orientation).
- c-axis orientation of the L i (N b x T a ! _ x) 0 3 thin film, the X-ray diffraction pattern, the peak of the (0 0 6) 2 0 is 3 9 °.
- High c-axis orientation means that the value of "c" is 50% or more.
- one electrode is provided around a polycrystalline diamond substrate, and a diamond substrate is used as the other electrode, and a bias voltage is applied between the electrode and the substrate. It is characterized in that the film is formed while being formed.
- a thin film of L i (Nb x T ai — x ) 0 3 (0 ⁇ x 1) can be formed while performing the polarization process, and an L film having excellent piezoelectric characteristics can be formed.
- i (Nb x T ai — x ) 0 3 (where 0 x ⁇ 1) A thin film can be formed on a diamond substrate.
- the one electrode is arranged in parallel with the film forming surface of the diamond substrate.
- the direction of L i (N b x T a ! _ X) 0 3 thin film the c-axis of the electric field deposition are parallel, easily uniformly polarized in the plane of the diamond substrate Become.
- the distance between the one electrode and the diamond substrate is desirably 20 mm or less in order to increase the electric field.
- the film-forming surface of the substrate is arranged perpendicular to the flight direction of the emitted particles.
- the diamond substrate may be arranged substantially parallel to the flight direction.
- the one electrode is arranged so as to be parallel to the diamond substrate.
- the diamond substrate becomes so-called shadows, and the deposition rate is significantly reduced, or the effect of not passing through one of the electrodes is reduced.
- the one electrode is formed by stretching a metal wire in a mesh shape or an interdigital shape. With such a shape, the particles emitted by the laser ablation can pass through the electrode, so that an arbitrary arrangement such as disposing the electrode between the target and the diamond substrate in the film forming apparatus can be used.
- the electrode can be placed at a location. When the diamond substrate and the electrode are arranged substantially in parallel to the flight direction of the particles, a metal plate may be used.
- the laser ablation method has the following advantages over other film forming methods such as the sputtering method.
- diamond substrate is exposed to an oxygen plasma (but, O x ⁇ l) L i (Nb x T ai _ x) 0 3 without the surface being damaged to be able to form a thin film, the impurity it contamination is small, it is excited because power density is higher available active L i (Nb x Ta x _ x) 0 3 in the film formation, and the like can be freely adjusted deposition rate. Due to the advantages of these laser ablation, the orientation and surface state of diamond on the diamond substrate, and the effect of the electric field, Li (Nb x T a! _ X ) 0 3 ( However, it seems that 0 x 1) thin film can be formed.
- O x ⁇ l L i (Nb x T ai _ x) 0 3
- FIG. 1 shows an outline of one embodiment of the laser ablation device of the present invention. -.
- Figure 2 shows the X-ray diffraction pattern of the L i Nb0 3 thin film formed in Example 1.
- Figure 3 shows the mouth Tsu King curves L i N b 0 3 thin film formed in Example 1.
- Figure 4 shows the X-ray diffraction pattern of the L i Nb0 3 thin film formed in Example 1.
- Figure 5 shows a mouth Tsu King curves L i N b 0 3 thin film formed in Example 1.
- the temperature and the target of the diamond base material in the present invention L i / Nb x T a! Shows the range of combinations of _ x ratio
- Figure 7 shows the X-ray diffraction pattern of the L i Nb_ ⁇ 3 thin film formed in Example 5.
- Figure 8 shows the X-ray diffraction pattern of the L i Nb_ ⁇ 3 thin film formed in Example 5.
- FIG. 9 shows an outline of another embodiment of the laser ablation device of the present invention.
- FIG. 10 shows an outline of another embodiment of the laser ablation apparatus of the present invention.
- FIG. 11 shows the SAW filter characteristics obtained in Example 6.
- FIG. 12 shows a comb electrode used for evaluation in the present invention.
- the inventors have proposed that, among the thin films of Li (Nb x Ta! _ 0 ) 0 3 (0 ⁇ 0 ⁇ 1), which are piezoelectric thin films, In order to form a piezoelectric thin film, it has been found that it is only necessary to use a diamond substrate in which the diamond of the diamond substrate is oriented (110) using a laser ablation method and the surface is polished to a mirror surface.
- the (1 10) orientation of the diamond substrate is preferably 15% or more, as evaluated by the aforementioned V ( ! 0). More preferably, it is at least 40%.
- the diamond substrate it is expedient to use polycrystalline diamond produced by a gas phase synthesis method.
- the vapor phase synthesis of diamond can be carried out by a conventionally known method such as a microwave plasma method and a thermal filament method under the condition of (110) orientation.
- a microwave plasma method By changing the synthesis conditions of diamond, diamonds with (1 1 1) or (100) orientation can be obtained.
- L i is larger than that of (1 10) oriented diamond.
- (Nb x T a - x) 0 3 was found that c-axis orientation Ya piezoelectric characteristics of the thin film is poor.
- the substrate used in the vapor phase synthesis of diamond is not particularly limited as long as diamond can be synthesized, but an Si wafer is generally used.
- the diamond surface after synthesis is mirror-finished using a diamond grindstone. At this time, it is desirable to perform mirror polishing until the surface roughness of the diamond surface becomes 0.1 l / im or less in Ry.
- an amorphous layer having a thickness of 1 nm or more and 50 nm or less is formed on the surface of the diamond by the mirror finishing.
- the L i (Nb x T ai — x ) 0 3 thin film is preferentially c-axis oriented, and the poly crystal L i (Nb x T a! _ X ) 0 (3)
- the best piezoelectric characteristics can be obtained as a thin film.
- the surface of the polycrystalline diamond is not covered with the amorphous layer, since the surface of the polycrystalline diamond has a (1 10) oriented diamond crystal having another crystal orientation, L i ( Nb x Ta! _ X) 0 3 crystal orientation of the growth of the thin film, it is difficult to receive the influence of the crystal orientation of the (1 10) other than the diamond surface to obtain a good c-axis orientation.
- the amount of the diamond abrasive grains on the diamond grindstone surface protruding from the grindstone surface is controlled. This is very important. If the protrusion amount is large, the diamond abrasive grinds the diamond surface of the polycrystalline diamond substrate so as to scratch it, so that it is difficult to form an amorphous layer.
- An appropriate protrusion amount is about 2 ⁇ .
- the laser used for laser ablation can be used as long as it has a wavelength of 360 nm or less and has a laser width of 1 / sec or less.
- Such lasers there are such Ar F and F 2 excimer laser, it is desirable that the laser light density is 1 J / cm 2 or more, K r F excimer laser oxygen can activate wavelength 248 nm is optimal It is.
- a laser frequency of about 1 to 5 OHz is suitable.
- Laser ablation conditions may be such that the temperature of the polycrystalline diamond substrate is 400 ° C. or higher. However, if the temperature is 1000 ° C. or higher, the diamond is deteriorated.
- the atmosphere is oxygen, ozone, N 2 0., oxidizing gas is preferably made of N0 2, atmospheric pressure is in the range of 0. 1 to 100 P a are suitable.
- the atmospheric pressure is less than 0.1 Pa, the amount of oxygen in the piezoelectric thin film is insufficient, so that the piezoelectric thin film cannot be formed. Further, on the oxygen when the pressure exceeds 1 OOP a becomes excessive, the energy of L i (Nb x T a!
- the distance between the polycrystalline diamond substrate and the target is preferably between 10 mm and 1000 mm.
- the temperature is preferably 400 ° C. or more and 100 ° C. or less.
- L i Nb x T a J — x Crystallization of the deficient phase proceeds, and the L i (Nb x T a J — x ) O 3 thin film tends to become amorphous. If L i / N b x T a ! _ X ratio increases, i.e. L i increases, Dari amorphous layer made form, L i excess phase such as L i 3 N b 0 4 is formed. Therefore, L i ZN b x T a x ratio of the raw material target is 0.9 or more, 1.5 or less. If L i N b x T a x ratio exceeds 1.
- L i atom Higher temperature of the polycrystalline diamond substrate comprises more evaporation Shasuku, in the thin film formed on the polycrystalline Daiyamondo substrate
- the Li amount can be controlled in the range of 0.8 to 1.1.
- Li ZNb x Ta! The upper limit of the _x ratio is 2.5. Therefore, temperature and L i / Nb x T a J _ x ratio of the polycrystalline diamond substrate is preferably in the range as shown in FIG.
- Raw material target is, it is preferable to use a sintered body of L i (N b x T a ! _ X) 0 3.
- a sintered body made of a mixture of Li 2 C0 3 Li 2 O may be used.
- the composition ratio L i Z mixture (N b x T a x _ x) is 0.9 or more 2.5 or less is preferably in the range of.
- any electrode When laser ablation is performed while applying a bias voltage, any electrode may be used as long as it has conductivity, but a metal is preferable in terms of handling. Further, in order to perform the polarization treatment uniformly, the area of the electrode may be at least the same as or larger than the area of the polycrystalline diamond substrate. There is no particular upper limit, but the upper limit is naturally determined by the size of the equipment used.
- the piezoelectric characteristics are excellent. This is because the surface of Li (Nb x Ta! _ X ) 0 3 thin film is in a metastable state, and Li atoms with high mobility move in accordance with the electric field during crystallization. This is because polarization processing can be sufficiently performed even with an electric field smaller than the stable state.
- the electric field is generated by placing a DC power supply between the polycrystalline diamond substrate and the electrode and applying a potential to the electrode.
- the electric field that can be polarized may be 10 to 1000 VZcm between the diamond substrate and the electrode. If less than 1 OVZcm, no polarization treatment is performed. Further, 1000 exceeds VZcm, than the electrodes to discharge, L i (Nb x Ta! _ X) to form 0 3 thin film leads to deterioration of the monitor quality impurities liable to be contaminated. However, since electric discharge is likely to occur in a reduced-pressure atmosphere, the electric field is more preferably 100 to 300 VZcm for suppressing the electric discharge and increasing the efficiency of the polarization treatment.
- L i (Nb x T a! _ X) 0 3 thin film formed as described above on the diamond substrate is a c-axis orientation.
- the orientation was evaluated by the X-ray rocking pattern method. Details of the evaluation method are disclosed, for example, in Japanese Patent Application Laid-Open No. 8-32398. In this way, indicating that good orientation of the higher standard deviation ⁇ of the measured rocking curve is less L i (Nb x T aj _ x) 0 3.
- the ⁇ value of L i (N b x T a ! _ X) 0 3 thin film of the present invention was less than 2 °.
- Figure 1 shows an overview of the device.
- the raw material target 4 is irradiated with the laser light of the excimer laser 11 through the lens 2 and the window 3 to instantaneously care the raw material target.
- a piezoelectric thin film is formed on the diamond substrate 5.
- Raw material target was used sintered body (size 2 Ommd) X 5mm) for the L i Nb_ ⁇ 3 as a raw material.
- the composition ratio of LiZNb in the target was 1.0.
- the polycrystalline diamond substrate is formed by forming about 25 ⁇ of polycrystalline diamond on single crystal Si by hot filament vapor phase synthesis under the condition of (1 10) orientation, and then the amount of diamond abrasive protrusion on the diamond surface was mirror-polished using a diamond whetstone controlled to about 2 ⁇ m.
- the surface roughness of the mirror-finished diamond was 1 and 0.08 ⁇ . Observation of the outermost surface of the diamond substrate ( ⁇ ) by transmission electron diffraction showed no diffraction image, confirming that an amorphous layer had been formed.
- a polycrystalline diamond substrate (B) was prepared by mirror-polishing polycrystalline diamond synthesized in the same manner using a diamond whetstone with a diamond abrasive protrusion of 5 ⁇ m or more.
- a diffraction image was observed, and it was confirmed that no amorphous layer was present.
- the surface roughness of the diamond substrate (B) is 0.08 ⁇ in Ry.
- laser light r F excimer laser is irradiated to the sintered body target, in an oxygen gas atmosphere to deposit a L i NbO 3 thin film to the two substrates.
- the output of the lasers had use is 750 meters J, the energy density of the laser beam at 4 J / cm 2, the frequency is 5 Hz.
- the temperature of the diamond substrate was 500 ° C, the distance between the target and the diamond substrate was 80 mm, the reaction pressure was 13 Pa, and the reaction time was 30 minutes.
- FIG. 2-5 The obtained L i Nb 0 3 X-ray diffraction pattern of the thin film "emissions and mouth Tsu King curves are shown in Figure 2-5.
- Figure 2 and Figure 3 are those that used a diamond base material (A)
- FIG. 4 and FIG. 5 is one using a diamond base material (B).
- L i Nb0 3 thin film obtained is c-axis oriented, gamma c was very good as 100%.
- the asperity value was good at 1.13 °, and from Fig. 4 and Fig.
- Example 2 The same device as in Example 1 was used.
- Raw target using sintered body (size 2 ⁇ X 5mm) as a raw material a mixture of L i NbO 3 and L i 2 CO 3.
- the composition ratio of Li / Nb of the target was set to 1.0.
- polycrystalline diamond was formed on a single crystal Si to a thickness of 25 m by changing the orientation conditions by the hot-filament gas phase synthesis method, and the diamond surface was mirror-finished.
- Table 1 shows the values of y (ii), which indicate the surface roughness and orientation of the diamond after mirror finishing.
- the outermost surface of the diamond substrate was observed by a transmission electron diffraction method as in Example 1, and it was confirmed that an amorphous layer was formed.
- Example 1 By using the raw material target and polycrystalline Daiyamondo substrate as described above, using the same laser as in Example 1, was on an oxygen gas atmosphere polycrystalline diamond substrate is deposited L i Nb0 3 thin film. Laser ablation conditions were the same as in Example 1. Table 1 shows the ⁇ value of the formed Li NbO 3 thin film measured by the X-ray diffraction pattern method and the Li ZNb ratio of the thin film.
- Example 2 The same device as in Example 1 was used.
- a raw material target a sintered body (size 2 Omm ⁇ i> X 5 mm) made of a mixture of Li Nb ⁇ 3 and Li 2 CO 3 was used.
- the composition ratio of Li / Nb of the target was adjusted so as to have the composition shown in Table 2.
- the polycrystalline diamond substrate is prepared by forming a polycrystalline diamond on a single crystal Si to the thickness shown in Table 1 under the orientation conditions shown in Table 1 by the hot-filament gas-phase synthesis method, and then mirror-finish the diamond surface. did.
- Table 2 shows the surface roughness of the diamond after mirror finishing.
- the outermost surface of the diamond substrate was observed by a transmission electron diffraction method as in Example 1, and it was confirmed that an amorphous layer had been formed.
- polycrystalline diamond substrate is deposited L i Nb0 3 thin film.
- Table 2 shows the L i ZNB ratio of laser ablation over Chillon condition as formed L i N b 0 3 ⁇ value was measured by X-ray diffraction pattern method of the thin film and formed film.
- No. 4 and No. 5 were measured by the X-ray diffraction method and found to be c-axis oriented. For No. 6, many fine particles are present on the surface of the obtained thin film. X-ray diffraction analysis revealed that the sample was amorphous without crystallization. The thin film of No. 7 was very similar to the thin film of No. 4, but the peaks of the (012) and (104) orientations were strongly determined by X-ray diffraction, and the c-axis orientation was not observed. Thin No 8, which had been the c-axis orientation, the orientation of ⁇ values 2. 1 ° and i N b 0 3 is, o New was used (1 10) oriented polycrystalline diamond substrate 4 was not better than the thin film. Example 4
- Example 2 The same device as in Example 1 was used.
- the composition ratio of the target L i / ⁇ a of No 7 was adjusted to so that such a composition shown in L i T a 0 3 and L i 2 C0 3 pine and mixed 3.
- Polycrystalline diamond substrate is a hot filament on single crystal Si.
- Polycrystalline diamond is formed by vapor phase synthesis under the orientation conditions shown in Table 3 to the thickness shown in Table 3, and the diamond surface is mirror-finished. did.
- Table 3 shows the surface roughness of the diamond after mirror finishing.
- the outermost surface of the diamond substrate was observed by a transmission electron diffraction method as in Example 1, and it was confirmed that an amorphous layer had been formed.
- polycrystalline diamond substrate is deposited L i Ta0 3 thin film.
- Table 3 shows the ⁇ values measured by X-ray diffraction pattern method of L i T a 0 3 thin film formed with the conditions of the laser ablation over Chillon.
- the thin film of No 13 had many fine particles on its surface, and was found to be amorphous by X-ray diffraction measurement.
- the thin film of No. 14 had an appearance very similar to that of No. 9, but as a result of X-ray diffraction measurement, in addition to the peak derived from diamond, 23.76 °, 32.88 °, 39-30 ° A peak was observed at This, L i T a 0 3 thin film plane index (012), (104), (00 6) corresponds to revealed that no c-axis oriented.
- Example 2 The same device as in Example 1 was used.
- a sintered body size 2 ⁇ X 5 mm
- raw material 1 and raw material 2 shown in Table 4 were adjusted to have the target composition ratio shown in Table 4, and a mixture was used as the raw material.
- a polycrystalline diamond substrate was formed on a single crystal Si by hot filament vapor phase synthesis method in which polycrystalline diamond was formed at about 25 / zm under the condition of (110) orientation, and the diamond surface was mirror-finished.
- the surface roughness of the mirror-finished diamond was Ry O. 08 / xm.
- the outermost surface of the diamond substrate was observed by a transmission electron diffraction method in the same manner as in Example 1, and it was confirmed that an amorphous layer was formed.
- Example 4 By using the raw material target and polycrystalline diamond substrate as described above, using the same laser as in Example 1, in an oxygen gas atmosphere on the polycrystalline diamond substrate is deposited L i N b0 3 thin film.
- the laser ablation conditions other than the substrate temperature and the reaction time are the same as in Example 1.
- Table 4 shows the temperature conditions of the diamond substrate and the composition of the thin film obtained by emission spectroscopy of the formed Li NbO 3 thin film. The reaction time is 10 minutes. Table 4
- Figure 7 shows the X-ray diffraction pattern of the thin film obtained in No. 15. From this figure, L i Nb_ ⁇ 3 thin film obtained we were are L i Nb0 3 single phase, it is Ru determine that c-axis oriented. Further, when the composition of the obtained thin film was examined by emission spectroscopy, the L i ZNb ratio was 1.01, which was close to the stoichiometric composition. A thin film of No 16 was X-ray diffraction analysis was L i Nb0 3 single phase. Further, when the composition of the obtained thin film was examined by emission spectroscopy, the LiZNb ratio was 1.02. Figure 8 shows the X-ray diffraction pattern of the thin film obtained in No. 17.
- L i Nb 0 3 thin film obtained is a L i Nb0 3 single phase, (104) peaks of observed, it is understood that poor c-axis orientation. Further, when the composition of the obtained thin film was examined by emission spectroscopy, the Li / Nb ratio was 1.09. The thin film obtained in No. 18 was measured by X-ray diffraction and found to be amorphous without being crystallized. Emission spectroscopy analysis showed that the LiZNb ratio was 1.66, which is significantly different from the stoichiometric composition. If the L i / Nb ratio of the polycrystalline diamond substrate and the target in the range shown in FIG. 6 as described above, L i ZNB ratio L i Nb O 3 thin film is formed, 0.80 or more, 1 .10 or less, indicating that a thin film having excellent orientation can be obtained.
- FIG. 9 shows an outline of one embodiment of the present invention when a bias voltage is applied.
- Electrode 7 is parallel to diamond substrate between raw material target 4 and diamond substrate 5 was placed.
- Raw target using sintered body (size 20 mm * X 5mm) to a raw material L i Nb0 3 powder.
- the composition ratio of LiZNb in the target is 1.0.
- the electrode used was a tungsten wire having a diameter of 0.15 mm fixed to a stainless steel frame and stretched vertically and horizontally at 2 mm intervals.
- a diamond substrate was formed on a single crystal Si by hot filament vapor phase synthesis method using polycrystalline diamond with a thickness of about 25 ⁇ under the condition of (110) orientation, and the diamond surface was mirror-polished.
- the surface roughness of the diamond after mirror finishing was Ry O.
- the outermost surface of the diamond substrate was observed by a transmission electron diffraction method as in Example 1, and it was confirmed that an amorphous layer had been formed.
- the diamond substrate and electrodes were arranged in parallel with the raw material target.
- the K r F excimer one The one first laser light having a wavelength of 248 nm through a lens 2 and the window 3 by irradiating the sintered body target, is deposited L i Nb_ ⁇ 3 thin film on board with an oxygen gas atmosphere was.
- the electrode potential was 140 V
- the diamond substrate potential was 0 V (ground).
- the distance between the electrode and the substrate is 6 mm
- the electric field between the electrode and the substrate is 23'3 VZcm.
- the substrate temperature was 530 ° C and the reaction time was 6 minutes. Other conditions are the same as in the first embodiment.
- a Li Nb ⁇ 3 thin film was synthesized on a diamond substrate.
- ⁇ value of L i N b 0 3 thin film obtained it was is 1.
- a 3.2 m-cycle comb-shaped electrode (inter-digital) as shown in Fig. 12 was formed on the formed Li NbO 3 thin film by a photolithography process.
- IDT IDT Transducer
- Example 7 Under the same conditions as in Example 5 for comparison, to form a L i N b 0 3 thin film without applying an electric field to the electrode and the substrate. Similarly forms form the ID T and L i N b 0 3 thin film in Example 5 was formed, was evaluated SAW filter characteristic, SAW filter characteristics can not be obtained, bad L i Nb0 3 thin film piezoelectric properties formed It turned out that it was done.
- Example 7
- Example 5 The same apparatus, raw material target, electrode, and diamond substrate as in Example 5 were used.
- the film forming conditions were the same as in Example 1 except for the potential of the electrode and the substrate.
- an electric field of 233 V / cm was applied between the electrode and the substrate.
- An IDT was formed on the thus formed LiNb ⁇ 3 thin film in the same manner as in Example 5, and the SAW filter characteristics were evaluated.
- the same results as in Example 5 were obtained, and the piezoelectric characteristics were excellent. it was found that L i Nb0 3 thin film was formed.
- Example 8 Example 8
- Example 5 The same apparatus, electrodes, diamond substrate, and film forming conditions as in Example 5 were used.
- Raw data one target is, L i (Nb.. 5 Ta.. 5) 0 3 powder was a sintered body obtained by sintering a.
- L i formed in this way (Nb 0. 5 T a. . 5) 0 3 ' was formed in the same manner as in the I DT as in Example 5 into a thin film, was evaluated SAW filter characteristic, Example 5 the same way results were obtained, excellent L i of the piezoelectric characteristics (Nb.. 5 Ta.. 5) 0 3 thin film was found to have been made form.
- Example 9 Example 9
- the apparatus shown in FIG. 10 was used.
- the diamond substrate 5 and the electrode 10 were arranged so as to be perpendicular to the raw material target 13. With this arrangement, the target particles emitted by the laser ablation do not pass through the electrode, so that the contamination of the formed thin film with impurities such as electrode components can be reduced.
- a raw material target a sintered body (size 2 ⁇ X 5 mm) using Li Nb O 3 powder as a raw material was used. The composition ratio of LiZNb in the target is 1.0.
- the electrode used was a 1 mm thick stainless steel plate.
- the diamond substrate was formed on a single crystal Si by hot filament vapor phase synthesis method using polycrystalline diamond with a thickness of about 25 ⁇ under the condition of (110) orientation, and the diamond surface was mirror-polished.
- the surface roughness of the diamond after mirror finishing was Ry O. 08 / im.
- the outermost surface of the diamond substrate was a transmission electrode in the same manner as in Example 1. Observation by the X-ray diffraction method confirmed that an amorphous layer had been formed.
- 1 wavelength 2 4811111: via r F lens 2 and the window 3 the laser beam of the excimer laser 1 irradiating the sintered body target were deposited L i Nb0 3 thin film diamond substrate in an oxygen gas atmosphere.
- the electrode potential was 140 V
- the diamond substrate potential was 0 V (ground).
- the distance between the electrode and the substrate is 6 mm
- the electric field between the electrode and the substrate is 233 V / cm.
- the substrate temperature was 530 ° C and the reaction time was 8 minutes. Other conditions are the same as in the first embodiment. In this case, the distance between the target and the diamond substrate indicates the distance between the target surface and the center of the diamond substrate.
- the orientation of the vapor phase synthetic polycrystalline diamond itself is
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Description
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Priority Applications (2)
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EP01982855A EP1375704A4 (en) | 2000-11-22 | 2001-11-19 | DIAMOND SUBSTRATE HAVING PIEZOELECTRIC THIN FILM AND METHOD OF MANUFACTURING THE SAME |
US10/362,890 US6794683B2 (en) | 2000-11-22 | 2001-11-19 | Diamond substrate having piezoelectric thin film, and method for manufacturing it |
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JP2000-355720 | 2000-11-22 | ||
JP2000355720 | 2000-11-22 | ||
JP2001-089535 | 2001-03-27 | ||
JP2001089535 | 2001-03-27 | ||
JP2001114056 | 2001-04-12 | ||
JP2001-114056 | 2001-04-12 | ||
JP2001-143104 | 2001-05-14 | ||
JP2001143104 | 2001-05-14 | ||
JP2001309289A JP4092900B2 (ja) | 2000-11-22 | 2001-10-05 | 圧電体薄膜を形成したダイヤモンド基板およびその製造方法 |
JP2001-309289 | 2001-10-05 |
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PCT/JP2001/010106 WO2002042527A1 (fr) | 2000-11-22 | 2001-11-19 | Substrat de diamant possedant un film mince piezo-electrique et procede de fabrication de celui-ci |
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US (1) | US6794683B2 (ja) |
EP (1) | EP1375704A4 (ja) |
JP (1) | JP4092900B2 (ja) |
WO (1) | WO2002042527A1 (ja) |
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US9362378B2 (en) | 2011-10-28 | 2016-06-07 | Indian Institute Of Technology Madras | Piezoelectric devices and methods for their preparation and use |
CN112532103A (zh) * | 2020-12-07 | 2021-03-19 | 上海大学 | 一种海洋能量收集装置 |
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JP4641009B2 (ja) * | 2006-07-07 | 2011-03-02 | 日本電信電話株式会社 | LiNbO3ターゲット及びLiNbO3薄膜の形成方法 |
US8456061B2 (en) * | 2011-01-25 | 2013-06-04 | Hewlett-Packard Development Company, L.P. | Architecture for piezoelectric MEMS devices |
JP2017079276A (ja) * | 2015-10-21 | 2017-04-27 | 株式会社リコー | 分極装置、分極方法 |
JP2021027375A (ja) * | 2019-07-31 | 2021-02-22 | 株式会社村田製作所 | 弾性波装置 |
Citations (3)
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JPH0578200A (ja) * | 1991-09-24 | 1993-03-30 | Asahi Chem Ind Co Ltd | 圧電体薄膜の合成方法 |
JPH0734223A (ja) * | 1993-07-14 | 1995-02-03 | Kawasaki Heavy Ind Ltd | 強誘電体薄膜の製造方法 |
JPH08154033A (ja) * | 1994-11-29 | 1996-06-11 | Sumitomo Electric Ind Ltd | ダイヤモンド基材および表面弾性波素子 |
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US4952832A (en) * | 1989-10-24 | 1990-08-28 | Sumitomo Electric Industries, Ltd. | Surface acoustic wave device |
JPH05319993A (ja) | 1991-09-20 | 1993-12-03 | Asahi Chem Ind Co Ltd | 圧電性LiNbO3薄膜 |
DE69420025T2 (de) * | 1994-03-25 | 2000-04-13 | Sumitomo Electric Industries | Orientierbares Material und Oberflächenwellenanordnung |
JP3344441B2 (ja) * | 1994-03-25 | 2002-11-11 | 住友電気工業株式会社 | 表面弾性波素子 |
JP3344442B2 (ja) | 1994-05-27 | 2002-11-11 | 住友電気工業株式会社 | 配向性材料および表面弾性波素子 |
JP3318920B2 (ja) * | 1994-05-10 | 2002-08-26 | 住友電気工業株式会社 | 表面弾性波素子 |
JP3282645B2 (ja) * | 1994-06-16 | 2002-05-20 | 住友電気工業株式会社 | 表面弾性波素子 |
US6127768A (en) * | 1997-05-09 | 2000-10-03 | Kobe Steel Usa, Inc. | Surface acoustic wave and bulk acoustic wave devices using a Zn.sub.(1-X) Yx O piezoelectric layer device |
JP4103421B2 (ja) * | 2001-03-28 | 2008-06-18 | セイコーエプソン株式会社 | 電子デバイス及び電子機器 |
-
2001
- 2001-10-05 JP JP2001309289A patent/JP4092900B2/ja not_active Expired - Fee Related
- 2001-11-19 US US10/362,890 patent/US6794683B2/en not_active Expired - Fee Related
- 2001-11-19 EP EP01982855A patent/EP1375704A4/en not_active Ceased
- 2001-11-19 WO PCT/JP2001/010106 patent/WO2002042527A1/ja active Application Filing
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JPH0578200A (ja) * | 1991-09-24 | 1993-03-30 | Asahi Chem Ind Co Ltd | 圧電体薄膜の合成方法 |
JPH0734223A (ja) * | 1993-07-14 | 1995-02-03 | Kawasaki Heavy Ind Ltd | 強誘電体薄膜の製造方法 |
JPH08154033A (ja) * | 1994-11-29 | 1996-06-11 | Sumitomo Electric Ind Ltd | ダイヤモンド基材および表面弾性波素子 |
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Cited By (3)
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---|---|---|---|---|
US9362378B2 (en) | 2011-10-28 | 2016-06-07 | Indian Institute Of Technology Madras | Piezoelectric devices and methods for their preparation and use |
US9882116B2 (en) | 2011-10-28 | 2018-01-30 | Indian Institute Of Technology Madras | Piezoelectric devices and methods for their preparation and use |
CN112532103A (zh) * | 2020-12-07 | 2021-03-19 | 上海大学 | 一种海洋能量收集装置 |
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US6794683B2 (en) | 2004-09-21 |
EP1375704A1 (en) | 2004-01-02 |
JP2003034592A (ja) | 2003-02-07 |
EP1375704A4 (en) | 2010-01-20 |
JP4092900B2 (ja) | 2008-05-28 |
US20030180984A1 (en) | 2003-09-25 |
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