WO2017085924A1 - 圧電体膜、圧電素子、および液体吐出装置 - Google Patents
圧電体膜、圧電素子、および液体吐出装置 Download PDFInfo
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- WO2017085924A1 WO2017085924A1 PCT/JP2016/004874 JP2016004874W WO2017085924A1 WO 2017085924 A1 WO2017085924 A1 WO 2017085924A1 JP 2016004874 W JP2016004874 W JP 2016004874W WO 2017085924 A1 WO2017085924 A1 WO 2017085924A1
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- 229910052719 titanium Inorganic materials 0.000 claims abstract description 9
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Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41J—TYPEWRITERS; SELECTIVE PRINTING MECHANISMS, i.e. MECHANISMS PRINTING OTHERWISE THAN FROM A FORME; CORRECTION OF TYPOGRAPHICAL ERRORS
- B41J2/00—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed
- B41J2/005—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed characterised by bringing liquid or particles selectively into contact with a printing material
- B41J2/01—Ink jet
- B41J2/135—Nozzles
- B41J2/14—Structure thereof only for on-demand ink jet heads
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41J—TYPEWRITERS; SELECTIVE PRINTING MECHANISMS, i.e. MECHANISMS PRINTING OTHERWISE THAN FROM A FORME; CORRECTION OF TYPOGRAPHICAL ERRORS
- B41J2/00—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed
- B41J2/005—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed characterised by bringing liquid or particles selectively into contact with a printing material
- B41J2/01—Ink jet
- B41J2/135—Nozzles
- B41J2/14—Structure thereof only for on-demand ink jet heads
- B41J2/14201—Structure of print heads with piezoelectric elements
- B41J2/14233—Structure of print heads with piezoelectric elements of film type, deformed by bending and disposed on a diaphragm
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41J—TYPEWRITERS; SELECTIVE PRINTING MECHANISMS, i.e. MECHANISMS PRINTING OTHERWISE THAN FROM A FORME; CORRECTION OF TYPOGRAPHICAL ERRORS
- B41J2/00—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed
- B41J2/005—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed characterised by bringing liquid or particles selectively into contact with a printing material
- B41J2/01—Ink jet
- B41J2/17—Ink jet characterised by ink handling
- B41J2/175—Ink supply systems ; Circuit parts therefor
-
- 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
-
- 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
- H10N30/20—Piezoelectric or electrostrictive devices with electrical input and mechanical output, e.g. functioning as actuators or vibrators
-
- 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
- H10N30/20—Piezoelectric or electrostrictive devices with electrical input and mechanical output, e.g. functioning as actuators or vibrators
- H10N30/204—Piezoelectric or electrostrictive devices with electrical input and mechanical output, e.g. functioning as actuators or vibrators using bending displacement, e.g. unimorph, bimorph or multimorph cantilever or membrane benders
- H10N30/2047—Membrane type
-
- 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
-
- 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
- H10N30/8548—Lead-based oxides
- H10N30/8554—Lead-zirconium titanate [PZT] based
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41J—TYPEWRITERS; SELECTIVE PRINTING MECHANISMS, i.e. MECHANISMS PRINTING OTHERWISE THAN FROM A FORME; CORRECTION OF TYPOGRAPHICAL ERRORS
- B41J2202/00—Embodiments of or processes related to ink-jet or thermal heads
- B41J2202/01—Embodiments of or processes related to ink-jet heads
- B41J2202/03—Specific materials used
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41J—TYPEWRITERS; SELECTIVE PRINTING MECHANISMS, i.e. MECHANISMS PRINTING OTHERWISE THAN FROM A FORME; CORRECTION OF TYPOGRAPHICAL ERRORS
- B41J2202/00—Embodiments of or processes related to ink-jet or thermal heads
- B41J2202/01—Embodiments of or processes related to ink-jet heads
- B41J2202/21—Line printing
Definitions
- the present invention relates to a piezoelectric film containing lead zirconate titanate, a piezoelectric element using the piezoelectric film, and a liquid ejecting apparatus.
- An actuator such as an ink jet recording head includes a piezoelectric element including a piezoelectric body having piezoelectricity that expands and contracts as the electric field application intensity increases and decreases, and an electrode that applies an electric field to the piezoelectric body. Yes.
- actuators have been miniaturized in combination with semiconductor process technology such as MEMS (Micro Electro-Mechanical Systems) technology in order to meet the demand for smaller devices.
- MEMS Micro Electro-Mechanical Systems
- high-precision processing using film formation, photolithography, or the like is possible, and therefore, studies are being conducted on actuators to reduce the thickness of piezoelectric materials.
- PZT lead zirconate titanate
- MPB morphotropic phase boundary
- Patent Document 1 in a piezoelectric element including a piezoelectric thin film in which a lead titanate layer having a columnar structure and a lead zirconate layer are stacked, the composition of lead titanate and lead zirconate in the piezoelectric thin film is expressed as MPB. It is described that the piezoelectric characteristics are improved by using the composition.
- a PZT piezoelectric film is doped with various donor ions having a valence higher than that of the ion to be substituted. Since the ion valence of Zr and Ti at the B site is tetravalent, the ion valences of V, Nb, Ta, Sb, Mo, W, etc. are 5 or more as the donor ions replacing the B site element. B site element is used. The amount replacing the B-site element was negligible. Specifically, in the case of Nb doping, it is about 0.2 to 0.025 mol% (see J. Am. Ceram. Soc, 84 (2001) 902 and Phys. Rev. Let, 83 (1999) 1347, etc.). The reason is that, if a large amount of doping is performed, the crystallization temperature rises to 800 ° C. or higher.
- Patent Document 2 is a ferroelectric thin film in which a dielectric material having a perovskite structure is formed on a substrate, and the dielectric material is an additive of a metal material other than Pb, Zr and Ti in PZT.
- the thin film is composed of a complex oxide, and the thin film includes layers having different Zr / Ti ratios, and has a first layer with a small Zr content on the substrate, and a Zr content with a large Zr content on the first layer. It has two layers.
- the quality of crystallinity changes depending on the compounding concentration of the additive, and even in a dielectric material whose piezoelectric characteristics change, if the compounding ratio of Zr is smaller than a predetermined ratio, the crystallinity becomes good.
- the blending ratio of is large up to a predetermined ratio, good piezoelectric characteristics are exhibited. Therefore, a combination of a first layer with a blending ratio with good crystallinity and a second layer with a blending ratio with high piezoelectric characteristics is used to combine A ferroelectric thin film having a predetermined thickness that exhibits characteristics can be formed with good crystallinity.
- a ferroelectric thin film exhibiting high piezoelectric characteristics is obtained by forming a ferroelectric thin film with good crystallinity on a substrate having a lower electrode layer formed on a substrate.
- a ferroelectric thin film with good crystallinity is obtained by forming a ferroelectric thin film with good crystallinity on a substrate having a lower electrode layer formed on a substrate.
- Patent Document 3 as a technique for suppressing high piezoelectric characteristics and cracking during film formation, a process of performing heat treatment after sputtering in an oxygen-free atmosphere and the amount of added metal doped into PZT are specified. is doing. However, in the method of Patent Document 3, heat treatment is required later, and it is difficult to control the amount of Pb because Pb evaporates at that time. In addition, the specified amount of added metal is better. Unable to bring out characteristics.
- JP 2012-99636 A International Publication No. 2012/124409 JP 2006-287254 A
- the piezoelectric film of the present invention is a piezoelectric film containing a perovskite oxide represented by the following general formula P.
- General formula P A includes at least Pb
- B includes at least Zr and Ti
- x and y satisfy 0.1 ⁇ x ⁇ 0.3 and 0 ⁇ y ⁇ 0.75x, respectively.
- ⁇ and z 3 are standard values, respectively, but these values may deviate from the standard values within a range in which a perovskite structure can be taken. Further, impurities may be contained within the range that the perovskite structure can be maintained.
- Y is preferably 0.2x ⁇ y ⁇ 0.4x.
- X is preferably 0.2 ⁇ x ⁇ 0.3.
- the piezoelectric film is preferably a columnar crystal film composed of a plurality of columnar crystals.
- the film thickness of the piezoelectric film is preferably 1 ⁇ m or more.
- the piezoelectric element of the present invention includes the piezoelectric film of the present invention and an electrode that applies an electric field to the piezoelectric film.
- the liquid ejection apparatus of the present invention includes the piezoelectric element of the present invention and a liquid ejection member provided integrally or separately from the piezoelectric element, and the liquid ejection member includes a liquid storage chamber in which liquid is stored; And a liquid discharge port through which liquid is discharged from the liquid storage chamber.
- the piezoelectric film of the present invention is represented by the general formula P as A 1 + ⁇ B 1-xy Nb x Ni y O z , A contains at least Pb, B contains at least Zr and Ti, and x and y are By satisfying 0.1 ⁇ x ⁇ 0.3 and 0 ⁇ y ⁇ 0.75x, respectively, high piezoelectric performance can be obtained even at low voltage driving.
- FIG. 1 is a schematic cross-sectional view showing an ink jet recording head which is an example of a liquid ejection apparatus having a piezoelectric element of the present invention.
- FIG. 2 is a schematic configuration diagram of an ink jet recording apparatus including the ink jet recording head of FIG. 3 is a partial top view of the ink jet recording apparatus of FIG.
- FIG. 4 is a diagram showing X-ray diffraction (XRD, X-ray diffraction) spectra of PZT films having different Nb doping amounts.
- FIG. 5 is a diagram showing an X-ray diffraction (XRD) spectrum of a PZT film doped with Nb and Ni in the present invention.
- FIG. 6 is a diagram showing the relationship between the Ni doping amount and -d31.
- FIG. 7 is a diagram showing the relationship between the drive voltage and -d31.
- the piezoelectric film of the present invention is a piezoelectric film containing a perovskite oxide represented by the following general formula P.
- General formula P A includes at least Pb
- B includes at least Zr and Ti
- x and y satisfy 0.1 ⁇ x ⁇ 0.3 and 0 ⁇ y ⁇ 0.75x, respectively.
- the piezoelectric film of the present invention is represented by the above general formula P, and in the general formula P, A (hereinafter also referred to as A site) contains at least Pb.
- a site contains at least Pb.
- Examples of the element that can replace the A site include at least one element selected from the group consisting of Ba, La, Sr, Bi, Li, Na, Ca, Mg, and K.
- the amount of the element substituting the A site is not particularly limited as long as it is within a range that can take a perovskite structure.
- B (hereinafter also referred to as B site) contains at least Zr and Ti.
- PZT-based perovskite oxides are said to exhibit high piezoelectric performance at and near the morphotropic phase boundary (MPB).
- MPB morphotropic phase boundary
- the rhombohedral system is formed when Zr is rich
- the tetragonal system is formed when Ti is rich
- the Zr / Ti molar ratio 55/45 is the boundary between the rhombohedral system and the tetragonal system, that is, MPB. It has become. Therefore, in the above general formula P, it is preferable that the MPB composition or close to it.
- Zr: Ti (molar ratio) is preferably in the range of 45:55 to 55:45.
- Nb is added to the B site.
- a PZT (hereinafter also referred to as PNZT) film to which Nb is added is known to have a high piezoelectric constant.
- the PNZT film exhibits a good hysteresis loop. Furthermore, the hysteresis loop is shifted to the positive voltage load side, and the polarization state has a direction from the beginning.
- the amount of Nb is increased, the piezoelectric performance can be improved.
- a perovskite structure cannot be formed, and a heterophase having no piezoelectricity called a pyrochlore phase is generated, which is not preferable.
- the Nb ratio x in the B site of the PNZT film of the present invention is preferably 0.1 ⁇ x ⁇ 0.3. By setting the Nb amount within this range, the piezoelectric performance during low-voltage driving can be improved.
- the Nb ratio x is more preferably 0.2 ⁇ x ⁇ 0.3.
- Ni is co-doped with Nb at the B site.
- the Ni ratio y in the B site is preferably 0 ⁇ y ⁇ 0.75x. By setting it as this range, the piezoelectric performance at the time of low voltage drive can be improved.
- the Ni ratio y is more preferably 0.2x ⁇ y ⁇ 0.4x.
- the piezoelectric film of the present invention containing the perovskite oxide represented by the general formula P can be formed by a non-thermal equilibrium process.
- a suitable film forming method of the piezoelectric film of the present invention sputtering method, plasma CVD method (Chemical Vapor Deposition), MOCVD method (Metal Organic Chemical Vapor Deposition), firing quench quench method, annealing
- the vapor deposition method include a quench method and a thermal spray quench method. Of these, the sputtering method is particularly preferable.
- the donor ions can be doped at a high concentration.
- the target in the sputtering method, is A 1 + ⁇ B 1-xy Nb x Ni y O z , A includes at least Pb, B includes at least Zr and Ti, x And y can be produced by making the composition satisfy 0.1 ⁇ x ⁇ 0.3 and 0 ⁇ y ⁇ 0.75x, respectively. That is, since the amount of Nb and Ni can be easily manufactured by adjusting the target composition, there is no trouble at the time of film formation.
- ⁇ is normally 0, but Pb is an element that is easily reverse sputtered. If Pb is removed from the formed piezoelectric film, it adversely affects crystal growth. In many cases, the film is formed with an amount larger than the stoichiometric composition of PZT. In that case, depending on the reverse sputtering rate of Pb, the formed film may also become Pb rich. As long as there is no hindrance in the characteristics, Pb deficiency may be present. By setting the range of 0 ⁇ ⁇ ⁇ 0.2, a high-quality perovskite oxide film without Pb deficiency can be obtained.
- Ts is preferably 450 ⁇ Ts (° C.) ⁇ 650.
- the sputtering method is preferable because the formed perovskite oxide film has a columnar crystal film structure composed of a plurality of columnar crystals extending non-parallel to the substrate surface.
- the growth direction of the columnar crystals may be non-parallel to the substrate surface, and may be substantially vertical or oblique.
- the alignment film since the alignment film has a uniform crystal orientation, higher piezoelectric performance can be obtained.
- the piezoelectric film doped with the above-described ratio of Nb and Ni can be formed with a film thickness of 1 ⁇ m or more.
- the average column diameter of the plurality of columnar crystals forming the piezoelectric film is not particularly limited, and is preferably 30 nm or more and 1 ⁇ m or less. By setting the average column diameter of the columnar crystals within this range, it is possible to achieve good crystal growth and to obtain a piezoelectric film that can be patterned with high accuracy.
- the average column diameter of a columnar crystal here means the average value of the column diameters of all the columnar crystals in the horizontal direction at a certain position in the film thickness direction.
- FIG. 1 is a schematic cross-sectional view of an ink jet recording head which is an example of a liquid ejection apparatus having a piezoelectric element.
- the piezoelectric element 1 of this embodiment is an element in which a lower electrode 30, a piezoelectric film 40, and an upper electrode 50 are sequentially stacked on a substrate 20.
- the lower electrode 30 and the upper electrode 50 apply an electric field in the thickness direction.
- the piezoelectric film 40 is the piezoelectric film of the present invention.
- the lower electrode 30 is formed on substantially the entire surface of the substrate 20, and a piezoelectric film 40 having a pattern in which line-shaped convex portions 41 extending from the front side to the rear side in the drawing are arranged in a stripe shape is formed thereon.
- An upper electrode 50 is formed on the portion 41.
- the pattern of the piezoelectric film 40 is not limited to the illustrated one, and can be changed as appropriate.
- the piezoelectric film 40 may be a continuous film.
- the piezoelectric film 40 is not a continuous film, but is formed by a pattern composed of a plurality of protrusions 41 separated from each other, so that the expansion and contraction of the individual protrusions 41 occurs smoothly, so that a larger displacement amount can be obtained. ,preferable.
- the substrate 20 is not particularly limited, and examples thereof include silicon, glass, stainless steel (SUS), yttrium-stabilized zirconia (YSZ), alumina, sapphire, silicon carbide and the like.
- a laminated substrate such as an SOI substrate in which a SiO 2 oxide film is formed on the surface of a silicon substrate may be used.
- the main component of the lower electrode 30 is not particularly limited , and examples thereof include metals or metal oxides such as Au, Pt, Ir, IrO 2, RuO 2, LaNiO 3, and SrRuO 3 , and combinations thereof.
- the main component of the upper electrode 50 is not particularly limited, and examples include materials exemplified for the lower electrode 30, electrode materials generally used in semiconductor processes such as Al, Ta, Cr, and Cu, and combinations thereof. .
- the thickness of the lower electrode 30 and the upper electrode 50 is not particularly limited, and is, for example, about 200 nm.
- the film thickness of the piezoelectric film 40 is not particularly limited and is usually 1 ⁇ m or more, for example, 1 ⁇ m to 5 ⁇ m.
- the film thickness of the piezoelectric film 40 is preferably 3 ⁇ m or more.
- the ink jet recording head (liquid ejecting apparatus) 2 generally includes an ink chamber (liquid storage chamber) 71 and an ink chamber on the lower surface of the substrate 20 of the piezoelectric element 1 having the above-described configuration.
- a plurality of ink chambers 71 are provided corresponding to the number and pattern of the convex portions 41 of the piezoelectric film 40.
- the electric field strength applied to the convex portion 41 of the piezoelectric element 1 is increased / decreased for each convex portion 41 to expand / contract, thereby controlling the ejection of ink from the ink chamber 71 and the ejection amount. Is called.
- a part of the substrate 20 may be processed into the diaphragm 60 and the ink nozzle 70.
- the substrate 20 is made of a laminated substrate such as an SOI substrate
- the substrate 20 is etched from the back side to form the ink chamber 71, and the vibration plate 60 and the ink nozzle 70 are formed by processing the substrate 20 itself.
- the piezoelectric element 1 and the ink jet recording head 2 of the present embodiment are configured as described above.
- FIG. 2 is a schematic configuration diagram of the ink jet recording apparatus.
- FIG. 3 shows a partial top view of the device. In order to facilitate visual recognition, the scale of the constituent elements is different from the actual one.
- an ink jet recording apparatus 100 includes a printing unit 102 having a plurality of ink jet recording heads (hereinafter simply referred to as “heads”) 2K, 2C, 2M, and 2Y provided for each ink color.
- An ink storage / loading unit 114 that stores ink to be supplied to each of the heads 2K, 2C, 2M, and 2Y, a paper feeding unit 118 that supplies the recording paper 116, and a decurl that removes curl of the recording paper 116.
- the suction belt conveyance unit 122 that is disposed to face the nozzle surface (ink ejection surface) of the printing unit 102 and conveys the recording paper 116 while maintaining the flatness of the recording paper 116, and the printing unit 102.
- a print detection unit 124 that reads a print result and a paper discharge unit 126 that discharges printed recording paper (printed matter) to the outside are roughly configured.
- Each of the heads 2K, 2C, 2M, and 2Y forming the printing unit 102 is the ink jet recording head 2 of the above embodiment.
- a cutter 128 is provided at the subsequent stage of the decurling unit 120, and the roll paper is cut into a desired size by this cutter.
- the cutter 128 includes a fixed blade 128A having a length equal to or larger than the conveyance path width of the recording paper 116 and a round blade 128B that moves along the fixed blade 128A.
- the fixed blade 128A is provided on the back side of the print.
- the round blade 128B is arranged on the printing surface side with the conveyance path interposed therebetween. In an apparatus using cut paper, the cutter 128 is unnecessary.
- the decurled and cut recording paper 116 is sent to the suction belt conveyance unit 122.
- the suction belt conveyance unit 122 has a structure in which an endless belt 133 is wound between rollers 131 and 132, and at least portions facing the nozzle surface of the printing unit 102 and the sensor surface of the printing detection unit 124 are horizontal ( Flat surface).
- the belt 133 has a width that is wider than the width of the recording paper 116, and a plurality of suction holes (not shown) are formed on the belt surface.
- a suction chamber 134 is provided at a position facing the nozzle surface of the print unit 102 and the sensor surface of the print detection unit 124 inside the belt 133 spanned between the rollers 131 and 132. The suction chamber 134 is sucked by the fan 135 to make a negative pressure, whereby the recording paper 116 on the belt 133 is sucked and held.
- the belt 133 When the power of a motor (not shown) is transmitted to at least one of the rollers 131 and 132 around which the belt 133 is wound, the belt 133 is driven in the clockwise direction in FIG. 2 and is held on the belt 133.
- the recording paper 116 is conveyed from left to right in FIG.
- the belt cleaning unit 136 is provided at a predetermined position (an appropriate position other than the printing region) outside the belt 133.
- a heating fan 140 is provided on the upstream side of the printing unit 102 on the paper conveyance path formed by the suction belt conveyance unit 122.
- the heating fan 140 heats the recording paper 116 by blowing heated air onto the recording paper 116 before printing. Heating the recording paper 116 immediately before printing makes it easier for the ink to dry after landing.
- the printing unit 102 is a so-called full line type head in which line type heads having a length corresponding to the maximum paper width are arranged in a direction (main scanning direction) perpendicular to the paper feed direction (see FIG. 3).
- Each of the print heads 2K, 2C, 2M, and 2Y is a line-type head in which a plurality of ink discharge ports (nozzles) are arranged over a length that exceeds at least one side of the maximum-size recording paper 116 targeted by the ink jet recording apparatus 100. It consists of
- Heads 2K, 2C, 2M, and 2Y corresponding to the respective color inks are arranged in the order of black (K), cyan (C), magenta (M), and yellow (Y) from the upstream side along the feeding direction of the recording paper 116.
- K black
- C cyan
- M magenta
- Y yellow
- a color image is recorded on the recording paper 116 by ejecting the color ink from each of the heads 2K, 2C, 2M, and 2Y while conveying the recording paper 116.
- the print detection unit 124 includes a line sensor that images the droplet ejection result of the print unit 102 and detects ejection defects such as nozzle clogging from the droplet ejection image read by the line sensor.
- a post-drying unit 142 composed of a heating fan or the like for drying the printed image surface is provided at the subsequent stage of the print detection unit 124. Since it is preferable to avoid contact with the printing surface until the ink after printing is dried, a method of blowing hot air is preferred.
- a heating and pressurizing unit 144 is provided to control the glossiness of the image surface.
- the heating and pressurizing unit 144 presses the image surface with a pressure roller 145 having a predetermined uneven surface shape while heating the image surface, and transfers the uneven shape to the image surface.
- the printed matter obtained in this manner is outputted from the paper output unit 126. It is preferable that the original image to be printed (printed target image) and the test print are discharged separately.
- a selection means (not shown) for switching the paper discharge path in order to select the prints of the main image and the prints of the test print and send them to the discharge units 126A and 126B. Is provided.
- a cutter 148 including a fixed blade 148A and a round blade 148B is provided to separate the test print portion.
- the ink jet recording apparatus 100 is configured as described above.
- a 10 nm thick Ti adhesion layer and a 300 nm thick Ir lower electrode are sequentially stacked on an SOI (Silicon on Insulater) substrate having a SiO 2 film formed on the surface of a 25 mm square (100) silicon substrate.
- SOI Silicon on Insulater
- a prepared electrode-attached substrate was prepared.
- An area that can be evaluated with a cantilever was previously provided in the substrate for piezoelectric constant evaluation.
- the electrode-attached substrate is placed in an RF sputtering apparatus, and the Zr / (Zr + Ti) in the target is used under conditions of a vacuum degree of 0.3 Pa and an Ar / O 2 mixed atmosphere (O 2 volume fraction of 2.0%).
- the Nb-doped PZT piezoelectric film having a thickness of 3.0 ⁇ m was formed at a substrate temperature of 450 ° C., with the amount of Nb doped into the B site being 10%, 20%, and 30%.
- the Ni doping amount was varied by using a target in which the amount of Ni in the piezoelectric film was changed.
- a Pt upper electrode having a thickness of 100 nm was formed on the Nb-doped PZT film to obtain a piezoelectric element.
- the longitudinal direction of the cantilever corresponds to the (110) direction of the crystal of the Si wafer, and the thickness direction corresponds to the (100) direction.
- a sin wave drive voltage with a frequency of 1 kHz, 2 Vpp, and an offset voltage of ⁇ 1 V is applied between the upper electrode and the lower electrode, and a sin wave drive voltage is applied.
- the tip displacement was measured with a laser Doppler vibrometer to determine the displacement.
- Vpp is a potential difference between the highest value and the lowest value of the AC voltage waveform.
- the resonance frequency was calculated by changing the length of the cantilever, and the effective length L 0 was determined by combining with the actually measured value.
- the length L 0 was set, the tip displacement was calculated, and the piezoelectric constant ⁇ d31 when it matched with the measured value was obtained, and this was used as the piezoelectric constant of the PZT thin film.
- the structure used in the finite element method is Pt (0.3 ⁇ m) ⁇ PZT / Ir (0.3 ⁇ m) / Si, and the following values were used as parameter values. Since Si is an anisotropic material, the Young's modulus and Poisson's ratio used in the simulation calculation must correspond to the longitudinal direction of the cantilever.
- FIG. 6 shows the relationship between the Ni doping amount and the piezoelectric constant -d31 when the applied voltage is 2 Vpp (offset voltage -1 V) for the PZT films having Nb doping amounts of 10%, 20%, and 30%.
- FIG. 6 shows that doping with Ni improves the piezoelectric constant, but if the doping amount is too large, no improvement in characteristics is confirmed. This is presumably that when the amount of Ni was excessive, it was not taken into the crystal, and as a result of the segregation of Ni, the characteristics were lowered.
- FIG. 6 shows that the optimum Ni doping amount depends on the Nb doping amount.
- FIG. 7 shows the applied voltage (Vpp offset voltage ⁇ Vpp) for a PZT film with 4.6%, 4.2%, and 4.2% of Ni added to Nb doping amounts of 10%, 20%, and 30%, respectively. / 2) and the piezoelectric constant -d31. It can be seen that doping with Ni greatly improves the characteristics at low voltage. Doping Ni eliminates the need for a polarization process because the polarization directions of the crystals in the film are aligned. Therefore, even if the film is not subjected to a polarization process, high piezoelectric performance can be obtained at low voltage drive. It is thought that was made.
- the piezoelectric film of the present invention is preferable for a piezoelectric actuator mounted on an ink jet recording head, a magnetic recording / reproducing head, a MEMS device, a micro pump, an ultrasonic probe, and a ferroelectric element such as a ferroelectric memory. Available.
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Abstract
Description
本発明は上記事情に鑑みてなされたものであり、低電圧駆動時においても圧電性能が高い圧電体膜、圧電素子、および液体吐出装置を提供するものである。
すなわち、本発明の圧電体膜は、下記一般式Pで表されるペロブスカイト型酸化物を含む圧電体膜である。
A1+δB1-x-yNbxNiyOz・・・一般式P
Aは少なくともPbを含み、Bは少なくともZrおよびTiを含み、xおよびyは、それぞれ0.1≦x≦0.3および0<y≦0.75xを満たす。δおよびzは、それぞれδ=0およびz=3が標準値であるが、これらの値はペロブスカイト構造を取り得る範囲内で標準値からずれてもよい。また、ペロブスカイト構造が保持できる範囲内で不純物を含んでも差し支えない。
d314Vpp/d3120Vpp≧0.8
であることが好ましい。
本発明の圧電体膜は、下記一般式Pで表されるペロブスカイト型酸化物を含む圧電体膜である。
A1+δB1-x-yNbxNiyOz・・・一般式P
Aは少なくともPbを含み、Bは少なくともZrおよびTiを含み、xおよびyは、それぞれ0.1≦x≦0.3および0<y≦0.75xを満たす。δおよびzは、それぞれδ=0およびz=3が標準値であるが、これらの値はペロブスカイト構造を取り得る範囲内で標準値からずれてもよい。また、ペロブスカイト構造が保持できる範囲内で不純物を含んでも差し支えない。
本発明のPNZT膜のBサイト中のNb比率xは、0.1≦x≦0.3が好ましい。Nb量をこの範囲とすることで低電圧駆動時の圧電性能を向上させることができる。Nb比率xは、0.2≦x≦0.3がより好ましい。
上記一般式Pで表されるペロブスカイト型酸化物を含む本発明の圧電体膜は、非熱平衡プロセスにより成膜することができる。本発明の圧電体膜の好適な成膜方法としては、スパッタリング法、プラズマCVD法(Chemical Vapor Deposition)、MOCVD法(有機金属気相成長法,Metal Organic Chemical Vapor Deposition)、焼成急冷クエンチ法、アニールクエンチ法、および溶射急冷法などの気相成長法が挙げられる。中でもスパッタリング法が特に好ましい。
また、スパッタリング法を用いることによって、上記NbとNiが上記比率でドープされた圧電体膜を1μm以上の膜厚で成膜することができる。
図1を参照して、本発明の圧電素子、およびこれを備えた液体吐出装置の一例であるインクジェット式記録ヘッドの実施形態について説明する。図1に、圧電素子を有する液体吐出装置の一例であるインクジェット式記録ヘッドの概略断面図である。
上部電極50の主成分としては特に制限なく、下部電極30で例示した材料、Al、Ta、Cr、およびCu等の一般的に半導体プロセスで用いられている電極材料、ならびにこれらの組合せが挙げられる。
本実施形態の圧電素子1およびインクジェット式記録ヘッド2は、以上のように構成されている。
図2および図3を参照して、上記実施形態のインクジェット式記録ヘッド2を備えたインクジェット式記録装置の構成例について説明する。図2に、インクジェット式記録装置の概略構成図を示す。図3に、装置の部分上面図を示す。視認しやすくするため、構成要素の縮尺は実際のものとは異なる。
ロール紙を使用する装置では、図2のように、デカール処理部120の後段に裁断用のカッター128が設けられ、このカッターによってロール紙は所望のサイズにカットされる。カッター128は、記録紙116の搬送路幅以上の長さを有する固定刃128Aと、固定刃128Aに沿って移動する丸刃128Bとから構成されており、印字裏面側に固定刃128Aが設けられ、搬送路を挟んで印字面側に丸刃128Bが配置される。カット紙を使用する装置では、カッター128は不要である。
印字検出部124は、印字部102の打滴結果を撮像するラインセンサ等からなり、ラインセンサによって読み取った打滴画像からノズルの目詰まり等の吐出不良を検出する。
大きめの用紙に本画像とテスト印字とを同時に並列にプリントする場合には、固定刃148Aと丸刃148Bとからなるカッター148を設けて、テスト印字の部分を切り離す構成とすればよい。
インクジェット式記録装置100は、以上のように構成されている。
本発明は上記実施形態に限定されるものではなく、本発明の趣旨を逸脱しない範囲内において、適宜設計変更可能である。
成膜基板として、25mm角の(100)シリコン基板の表面にSiO2膜が形成されたSOI(Silicon on Insulater)基板上に、10nm厚のTi密着層と300nm厚のIr下部電極とが順次積層された電極付き基板を用意した。基板には、圧電定数評価のために、カンチレバーで評価できる領域を予め設けておいた。
本発明の圧電体膜では、図5に示すように、BサイトにNiをドープすることによりパイロクロア結晶の形成を抑制し、圧電特性のあるペロブスカイト結晶が形成されることがわかった。
PZT中のNi量は、XRF(X‐ray Fluorescence,蛍光X線分析法)により検出した。また、作製したPZT膜をXRFにより組成評価すると、Pbは以下の範囲の組成であった。
Pb/(Zr+Ti+Nb)=1.00~1.20
NbドープPZT膜上に100nm厚のPt上部電極を成膜し、圧電素子とした。カンチレバー形成領域において、各々幅=2mm、長さ=24mm程の短冊状に加工してカンチレバーを作製した。なお、カンチレバーの長手方向がSiウエハーの結晶の(110)方向に対応し、厚み方向は(100)方向に対応するようにした。
Si(110)方位:ヤング率YSi=169GPa、ポアソン比nSi=0.064
PZT:ヤング率YPZT=50GPa、ポアソン比nPZT=0.34
Ir(下部電極):ヤング率YIr=530GPa、ポアソン比nIr=0.26
Pt(上部電極):ヤング率YPt=168GPa、ポアソン比nPT=0.39
図6から、Niをドープすることで圧電定数が向上するが、ドープ量が多すぎると特性向上が確認されないことがわかる。これは、Ni量が多くなり過ぎると、結晶に取り込まれず、Niが偏析した結果、特性低下が引き起こされたと考えられる。
また、図6から、最適なNiドープ量がNbドープ量に依存していることがわかる。すなわち、Nbドープ量が10%から30%へと多くなるにしたがって、Niを全く添加しない場合と比較して添加による圧電定数の上昇率が大きい。これは、特に10V以下の低電圧駆動時に顕著であった。表1は図6に用いたデータを表にしたものである。
Niをドープすることで低電圧時の特性が大きく向上している様子がわかる。Niをドープすることによって、膜内での結晶の分極方向が揃うために分極処理が不要になり、そのため、分極処理を実施しない膜であっても、低電圧駆動時で高い圧電性能を得ることができたと考えられる。
図7から、駆動電圧20Vppおよびオフセット電圧-10Vでの圧電定数d3120Vppに対する、駆動電圧4Vppおよびオフセット電圧-2Vでの圧電定数d314Vppが、
d314Vpp/d3120Vpp≧0.8
であることがわかる。このことは、低電圧駆動時に分極方向が揃っており、分極処理が不要であることを示すものである。表2は図7に用いたデータを表にしたものである。
2、2K,2C,2M,2Y インクジェット式記録ヘッド(液体吐出装置)
20 基板
30、50 電極
40 圧電体膜
70 インクノズル(液体貯留吐出部材)
71 インク室(液体貯留室)
72 インク吐出口(液体吐出口)
100 インクジェット式記録装置
Claims (8)
- 下記一般式Pで表されるペロブスカイト型酸化物を含む圧電体膜。
A1+δB1-x-yNbxNiyOz・・・一般式P
Aは少なくともPbを含み、Bは少なくともZrおよびTiを含み、xおよびyは、それぞれ0.1≦x≦0.3および0<y≦0.75xを満たす。δおよびzは、それぞれδ=0およびz=3が標準値であるが、これらの値はペロブスカイト構造を取り得る範囲内で標準値からずれてもよい。 - 前記yが、0.2x≦y≦0.4xである請求項1記載の圧電体膜。
- 前記xが、0.2≦x≦0.3である請求項2記載の圧電体膜。
- 複数の柱状結晶からなる柱状結晶膜である請求項1から3いずれか1項記載の圧電体膜。
- 圧電体膜の膜厚が1μm以上である請求項1から4いずれか1項記載の圧電体膜。
- 請求項1から5いずれか1項記載の圧電体膜と、該圧電体膜に対して電界を印加する電極とを備えた圧電素子。
- 駆動電圧20Vppおよびオフセット電圧-10Vでの圧電定数d3120Vppに対する、駆動電圧4Vppおよびオフセット電圧-2Vでの圧電定数d314Vppが、
d314Vpp/d3120Vpp≧0.8
である請求項6記載の圧電素子。 - 請求項6または7記載の圧電素子と、該圧電素子に一体的にまたは別体として設けられた液体吐出部材とを備え、該液体吐出部材は、液体が貯留される液体貯留室と、該液体貯留室から外部に前記液体が吐出される液体吐出口とを有する液体吐出装置。
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EP4307870A1 (en) | 2022-07-13 | 2024-01-17 | FUJIFILM Corporation | Piezoelectric laminate and piezoelectric element |
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JP6392469B2 (ja) | 2018-09-19 |
US10217929B2 (en) | 2019-02-26 |
JPWO2017085924A1 (ja) | 2018-09-20 |
DE112016005244B4 (de) | 2019-12-24 |
DE112016005244T5 (de) | 2018-08-16 |
US20180254406A1 (en) | 2018-09-06 |
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