JP2014203840A - 圧電体膜および圧電体膜の製造方法 - Google Patents
圧電体膜および圧電体膜の製造方法 Download PDFInfo
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- JP2014203840A JP2014203840A JP2013076022A JP2013076022A JP2014203840A JP 2014203840 A JP2014203840 A JP 2014203840A JP 2013076022 A JP2013076022 A JP 2013076022A JP 2013076022 A JP2013076022 A JP 2013076022A JP 2014203840 A JP2014203840 A JP 2014203840A
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- piezoelectric film
- piezoelectric
- film
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- carbon
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- 239000013078 crystal Substances 0.000 claims abstract description 28
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000001301 oxygen Substances 0.000 claims abstract description 16
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 66
- 229910052799 carbon Inorganic materials 0.000 claims description 66
- 239000002245 particle Substances 0.000 claims description 45
- 239000002994 raw material Substances 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 21
- 238000004544 sputter deposition Methods 0.000 claims description 21
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- 238000001354 calcination Methods 0.000 description 6
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- 238000012360 testing method Methods 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 5
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- 239000010409 thin film Substances 0.000 description 4
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 230000001678 irradiating effect Effects 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000004931 aggregating effect Effects 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
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- 229910052736 halogen Inorganic materials 0.000 description 2
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- 238000003980 solgel method Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 229920005992 thermoplastic resin Polymers 0.000 description 2
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- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 206010021143 Hypoxia Diseases 0.000 description 1
- 241000877463 Lanio Species 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910004121 SrRuO Inorganic materials 0.000 description 1
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- 235000010724 Wisteria floribunda Nutrition 0.000 description 1
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- 150000004703 alkoxides Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
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- 229910052737 gold Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229910002076 stabilized zirconia Inorganic materials 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
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- 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
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- 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
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/49—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates
- C04B35/491—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates based on lead zirconates and lead titanates, e.g. PZT
- C04B35/493—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates based on lead zirconates and lead titanates, e.g. PZT containing also other lead compounds
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- C04B35/495—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
- C04B35/497—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates based on solid solutions with lead oxides
- C04B35/499—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates based on solid solutions with lead oxides containing also titanates
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- C23C14/08—Oxides
- C23C14/088—Oxides of the type ABO3 with A representing alkali, alkaline earth metal or Pb and B representing a refractory or rare earth metal
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- 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
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- 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
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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- C—CHEMISTRY; METALLURGY
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- 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
- C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
- C23C14/564—Means for minimising impurities in the coating chamber such as dust, moisture, residual gases
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- 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
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
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- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3251—Niobium oxides, niobates, tantalum oxides, tantalates, or oxide-forming salts thereof
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Abstract
Description
(d31)2/(ε×tanδ×1000)>3
を満たす圧電体膜を提供する。
(式中、x:鉛量、y:Nb量(Bサイトドープ量)、z:酸素量、a:Zr/Ti比であり、y>0.14である。x=1.0、z=3である場合が標準であるが、ペロブスカイト構造を取り得る範囲内でずれてもよい。)
圧電定数d31は、印加電圧に対する変位量を示すため、圧電定数d31が大きい程、電圧に対する変位量が大きくなる。比誘電率εは、物質に電界を印加したときに、物質中の原子がどの程度応答するかを示す物理量であり、比誘電率εが大きい程、多くの供給電流が必要になる。誘電損失tanδは、圧電体に交流電界を印加したときに生じる電気エネルギー損失の度合いを表わす定数であり、誘電損失tanδが大きい程、消費電力が大きくなる。したがって、上記式の数値が大きい程、効率の良い圧電体膜であることを意味する。
(式中、x:鉛量、y:Nb量(Bサイトドープ量)、z:酸素量、a:Zr/Ti比であり、y>0.14である。x=1.0、z=3である場合が標準であるが、ペロブスカイト構造を取り得る範囲内でずれてもよい。)
Nbのドープ量が多くなると、圧電体膜中にカーボンを取り込みやすくなり、消費電力が高くなる。本発明によれば、Nbのドープ量(y)が14%以上で、圧電体膜の膜厚が2μm以上であるカーボンを取り込みやすい圧電体膜において、圧電体膜中のカーボン量の指標として、カーボンを含み粒径200nm以上の析出粒子の数が1000個以下/μm2とする。このような構成とすることで、カーボン量の少ない圧電体膜とすることができ、高い圧電対数d31を有し、消費電力の少ない圧電体膜とすることができる。
(式中、x:鉛量、y:Nb量(Bサイトドープ量)、z:酸素量、a:Zr/Ti比であり、y>0.14である。x=1.0、z=3である場合が標準であるが、ペロブスカイト構造を取り得る範囲内でずれてもよい。)
本発明によれば、スパッタ法により製造される圧電体膜の原料ターゲットのカーボン濃度を200ppmとしたカーボン濃度の低い原料ターゲットを用いて圧電体膜の製造を行っているので、製造された圧電体膜のカーボン量を少なくすることができる。したがって、圧電体膜のカーボン量を少なくすることにより、比誘電率ε、誘電損失tanδを抑えることができ、供給電流、消費電力の抑えた圧電体膜を製造することができる。
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結晶構造を主成分とする圧電体膜である。
式中、x:鉛量、y:Nb量(Bサイトドープ量)、z:酸素量、a:Zr/Ti比であり、y>0.14である。x=1.0、z=3である場合が標準であるが、ペロブスカイト構造を取り得る範囲内でずれてもよい。
圧電体膜における消費電力は、印加電圧[V]をV、比誘電率[−]をε、誘電損失[−]をtanδとしたとき、ε×tanδ×V2に比例する。同じ圧電変位を得るためには、印加電圧は、圧電定数d31[pm/V]に反比例することから、(ε×tanδ)/(d31)2が消費電力の指標となる。すなわち、下記の式(B)の数値が高いほど効率の良い圧電体膜であることを意味する。なお、分母の1000については、数値を単純化するためにかけている。
本実施形態においては、式(B)の値を、3を超える数値とする。
上記式(P)で表されるペロブスカイト型結晶構造を主成分とする圧電体膜は、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、スパッタ法、プラズマCVD法、焼成急冷クエンチ法、アニールクエンチ法、および、溶射急冷法などが挙げられる。中でも、スパッタ法が特に好ましい。
Ts(℃)≧400・・・(1)、
−0.2Ts+100<Vs−Vf(V)<−0.2Ts+130・・・(2)、
10≦Vs−Vf(V)≦35・・・(3)
プラズマ空間Pの電位はプラズマ電位Vs(V)となる。通常、成膜基板Bは絶縁体であり、かつ、電気的にアースから絶縁されている。したがって、成膜基板Bはフローティング状態にあり、その電位はフローティング電位Vf(V)となる。ターゲットTと成膜基板Bとの間にあるターゲットの構成元素は、プラズマ空間Pの電位と成膜基板Bの電位との電位差Vs−Vfの加速電圧分の運動エネルギーを持って、成膜中の成膜基板Bに衝突すると考えられる。
図4を参照して、本発明に係る実施形態の圧電素子、およびこれを備えたインクジェット式記録ヘッド(液体吐出装置)の構造について説明する。図4はインクジェット式記録ヘッドの要部断面図である。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適宜異ならせてある。
図5を参照してインクジェット式記録ヘッド3(172M、172K、172C、172Y)を備えたインクジェット記録装置の構成例について説明する。図5は、装置全体図である。
給紙部112は、記録媒体124を処理液付与部114に供給する機構であり、当該給紙部112には、枚葉紙である記録媒体124が積層されている。給紙部112には、給紙トレイ150が設けられ、この給紙トレイ150から記録媒体124が一枚ずつ処理液付与部114に給紙される。
処理液付与部114は、記録媒体124の記録面に処理液を付与する機構である。処理液は、描画部116で付与されるインク中の色材(本例では顔料)を凝集させる色材凝集剤を含んでおり、この処理液とインクとが接触することによって、インクは色材と溶媒との分離が促進される。
描画部116は、描画ドラム(第2の搬送体)170、用紙抑えローラ174、およびインクジェット式記録ヘッド172M,172K,172C,172Yを備えている。
乾燥部118は、色材凝集作用により分離された溶媒に含まれる水分を乾燥させる機構であり、図4に示すように、乾燥ドラム(搬送体)176、および溶媒乾燥装置178を備えている。
定着部120は、定着ドラム184、ハロゲンヒータ186、定着ローラ188、およびインラインセンサ190で構成される。定着ドラム184の回転により、記録媒体124は記録面が外側を向くようにして搬送され、この記録面に対して、ハロゲンヒータ186による予備加熱と、定着ローラ188による定着処理と、インラインセンサ190による検査が行われる。
定着部120に続いて排出部122が設けられている。排出部122は、排出トレイ192を備えており、この排出トレイ192と定着部120の定着ドラム184との間に、これらに対接するように渡し胴194、搬送ベルト196、張架ローラ198が設けられている。記録媒体124は、渡し胴194により搬送ベルト196に送られ、排出トレイ192に排出される。
Nbのドーピング量、および、原料ターゲットのカーボン濃度を変更して、圧電体膜を成膜し、圧電特性を評価した。
Siウエハ上にスパッタ法により、下部電極として20nm厚のTi膜と150nm厚の(111)Ir膜とを順次成膜した。この下部電極上にNb−PZT圧電体膜を成膜した。Nb−PZT圧電体膜の総厚は2μmとした。
成膜装置:RFスパッタ装置(アルバック社製「強誘電体成膜スパッタ装置MPS型」)、
ターゲット:120mmφのPb1.3((Zr0.52Ti0.48)1−xNbx)O3焼結体、(なお、xは、ドープするNb量により変更する。Nbドープ量14%の場合x=0.12ターゲット、Nbドープ量18%の場合x=0.15ターゲット、Nbドープ量23%の場合x=0.20ターゲットを用いる。)
成膜パワー:500W、
基板/ターゲット間距離:60mm、
成膜圧力:0.3Pa、
成膜ガス:Ar/O2=97.5/2.5(モル比)。
Nbのドープ量を14%(比較例1、2)、20%(実施例2、比較例4)、23%(実施例3、比較例5)、成膜時の原料ターゲットのカーボン量を200ppm(比較例1、実施例2、3)、従来の原料の600ppm(比較例2、3、4、5)とした以外は実施例1と同様の方法により成膜した。また、参考例として、従来の高性能圧電バルク体として知られている、富士セラミック製、C92Hのデータについても記載する。
結果を図7に示す。比較例1、2で示すように、Nbのドープ量が14%の圧電体膜においては、原料ターゲットのカーボン濃度によらず、良質な圧電体膜を得ることができた。Nbが14%を超える圧電定数の良好な膜においては、従来のカーボン濃度である原料ターゲットを用いた比較例3〜5は、原料などから供給されるカーボンを取り込みやすく、比誘電率ε、誘電損失tanδが高くなった。比較例3〜5の圧電体膜は消費電力が高いと考えられる。原料ターゲットにカーボンン濃度が200ppmの低い材料を用いて成膜した実施例1〜3においては、圧電定数は、従来の原料ターゲット(カーボン濃度600ppm)で成膜した圧電体膜の数値を維持しつつ、比誘電率ε、誘電損失tanδを下げることができ、供給電流、消費電力を抑えることができた良好な膜を得ることができた。
≪試験例2≫
次に、試験例1で形成した実施例1〜3、比較例1〜5の圧電体膜について、圧電体膜表面の粒径200nm以上の析出粒子の数を調べた。析出粒子の数は、電子顕微鏡写真から単位面積あたりの析出粒子の個数を数えて確認した。結果を図8に示す。本発明においては、析出粒子の数が1000個以下/μm2であると比誘電率ε、誘電損失tanδを抑えることができることが確認できる。
Claims (8)
- 下記式(P)で表されるペロブスカイト型結晶構造を有する圧電体膜であって、
圧電定数d31[pm/V]、比誘電率ε[−]、誘電損失tanδ[−]としたとき、
(d31)2/(ε×tanδ×1000)>3
を満たす圧電体膜。
Pbx[(ZraTi1−a)1−yNby]Oz・・・(P)
(式中、x:鉛量、y:Nb量(Bサイトドープ量)、z:酸素量、a:Zr/Ti比であり、y>0.14である。x=1.0、z=3である場合が標準であるが、ペロブスカイト構造を取り得る範囲内でずれてもよい。) - 前記ペロブスカイト型結晶構造を構成する結晶が、(100)方向あるいは(001)方向を主成分とする請求項1に記載の圧電体膜。
- 前記圧電体膜の膜厚が2μm以上10μm以下である請求項1又は2に記載の圧電体膜。
- 前記式(P)中のyが、y≧0.18の範囲内にある請求項1から3のいずれか1項に記載の圧電体膜。
- 前記ペロブスカイト型結晶構造を構成する結晶が、柱状結晶である請求項1から4のいずれか1項に記載の圧電体膜。
- 下記式(P)で表されるペロブスカイト型結晶構造を有する圧電体膜であって、
前記圧電体膜の膜厚が2μm以上であり、かつ、前記圧電体膜の表面のカーボンを含み粒径200nm以上の析出粒子の数が1000個以下/μm2である圧電体膜。
Pbx[(ZraTi1−a)1−yNby]Oz・・・(P)
(式中、x:鉛量、y:Nb量(Bサイトドープ量)、z:酸素量、a:Zr/Ti比であり、y>0.14である。x=1.0、z=3である場合が標準であるが、ペロブスカイト構造を取り得る範囲内でずれてもよい。) - 前記圧電体膜の膜厚が3μm以上である請求項6に記載の圧電体膜。
- 下記式(P)で表されるペロブスカイト型結晶構造を有する圧電体膜の製造方法であって、
成膜する圧電体膜の膜組成に応じた組成であり、カーボン濃度が200ppm以下である原料ターゲットを用いて、スパッタ法により成膜を行う圧電体膜の製造方法。
Pbx[(ZraTi1−a)1−yNby]Oz・・・(P)
(式中、x:鉛量、y:Nb量(Bサイトドープ量)、z:酸素量、a:Zr/Ti比であり、y>0.14である。x=1.0、z=3である場合が標準であるが、ペロブスカイト構造を取り得る範囲内でずれてもよい。)
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JP2010182717A (ja) * | 2009-02-03 | 2010-08-19 | Fujifilm Corp | 圧電体とその製造方法、圧電素子、及び液体吐出装置 |
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JP5601899B2 (ja) * | 2010-06-25 | 2014-10-08 | 富士フイルム株式会社 | 圧電体膜および圧電素子 |
US8383048B2 (en) * | 2010-07-21 | 2013-02-26 | Schlumberger Technology Corporation | Microsensor for mercury |
JP5385930B2 (ja) * | 2011-02-22 | 2014-01-08 | 富士フイルム株式会社 | 超音波手術装置 |
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JP2006105964A (ja) * | 2004-09-13 | 2006-04-20 | Denso Corp | 圧電センサ |
JP2010087144A (ja) * | 2008-09-30 | 2010-04-15 | Fujifilm Corp | 鉛含有圧電膜およびその作製方法、鉛含有圧電膜を用いる圧電素子、ならびにこれを用いる液体吐出装置 |
JP2010182717A (ja) * | 2009-02-03 | 2010-08-19 | Fujifilm Corp | 圧電体とその製造方法、圧電素子、及び液体吐出装置 |
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JP2016152237A (ja) * | 2015-02-16 | 2016-08-22 | 三菱マテリアル株式会社 | Ptzt圧電体膜及びその圧電体膜形成用液組成物の製造方法 |
CN107431123A (zh) * | 2015-02-16 | 2017-12-01 | 三菱综合材料株式会社 | Ptzt压电膜及其压电膜形成用液体组合物的制造方法 |
JP2016157894A (ja) * | 2015-02-26 | 2016-09-01 | 三菱マテリアル株式会社 | PNbZT膜及びPNbZT膜形成用組成物の製造方法 |
WO2017135166A1 (ja) * | 2016-02-05 | 2017-08-10 | 富士フイルム株式会社 | 圧電素子 |
JPWO2017135166A1 (ja) * | 2016-02-05 | 2018-12-06 | 富士フイルム株式会社 | 圧電素子 |
US10388851B2 (en) | 2016-02-05 | 2019-08-20 | Fujifilm Corporation | Piezoelectric element |
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US20160020381A1 (en) | 2016-01-21 |
US20180130942A1 (en) | 2018-05-10 |
JP5943870B2 (ja) | 2016-07-05 |
WO2014162999A1 (ja) | 2014-10-09 |
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