US20020098333A1 - Piezoceramic device - Google Patents
Piezoceramic device Download PDFInfo
- Publication number
- US20020098333A1 US20020098333A1 US09/736,266 US73626600A US2002098333A1 US 20020098333 A1 US20020098333 A1 US 20020098333A1 US 73626600 A US73626600 A US 73626600A US 2002098333 A1 US2002098333 A1 US 2002098333A1
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- United States
- Prior art keywords
- ceramic
- cations
- positions
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- perovskite
- Prior art date
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- 239000010949 copper Substances 0.000 claims abstract description 43
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910052802 copper Inorganic materials 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 26
- 239000000919 ceramic Substances 0.000 claims description 113
- 150000001768 cations Chemical class 0.000 claims description 46
- 238000005245 sintering Methods 0.000 claims description 32
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 25
- 239000001301 oxygen Substances 0.000 claims description 25
- 229910052760 oxygen Inorganic materials 0.000 claims description 25
- 238000004519 manufacturing process Methods 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 23
- 239000011888 foil Substances 0.000 claims description 22
- 229910052751 metal Inorganic materials 0.000 claims description 19
- 239000002184 metal Substances 0.000 claims description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 15
- 239000001257 hydrogen Substances 0.000 claims description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims description 15
- 239000011230 binding agent Substances 0.000 claims description 11
- MYLBTCQBKAKUTJ-UHFFFAOYSA-N 7-methyl-6,8-bis(methylsulfanyl)pyrrolo[1,2-a]pyrazine Chemical compound C1=CN=CC2=C(SC)C(C)=C(SC)N21 MYLBTCQBKAKUTJ-UHFFFAOYSA-N 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 230000002829 reductive effect Effects 0.000 claims description 9
- 239000000654 additive Substances 0.000 claims description 8
- 230000008018 melting Effects 0.000 claims description 8
- 238000002844 melting Methods 0.000 claims description 8
- 238000006467 substitution reaction Methods 0.000 claims description 8
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 7
- 150000002910 rare earth metals Chemical class 0.000 claims description 7
- 229910052726 zirconium Inorganic materials 0.000 claims description 7
- 229910052758 niobium Inorganic materials 0.000 claims description 6
- 229910052706 scandium Inorganic materials 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 6
- 229910052715 tantalum Inorganic materials 0.000 claims description 6
- 229910052738 indium Inorganic materials 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 238000010030 laminating Methods 0.000 claims description 4
- 229910052747 lanthanoid Inorganic materials 0.000 claims description 4
- 150000002602 lanthanoids Chemical class 0.000 claims description 4
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- 230000000996 additive effect Effects 0.000 claims description 3
- 239000011575 calcium Substances 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- 229910052788 barium Inorganic materials 0.000 claims description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052797 bismuth Inorganic materials 0.000 claims description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- 229920003009 polyurethane dispersion Polymers 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims description 2
- 229910052712 strontium Inorganic materials 0.000 claims description 2
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 claims 3
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 claims 3
- 239000011261 inert gas Substances 0.000 claims 2
- 229910020289 Pb(ZrxTi1-x)O3 Inorganic materials 0.000 claims 1
- 229910020273 Pb(ZrxTi1−x)O3 Inorganic materials 0.000 claims 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 7
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 15
- 238000009833 condensation Methods 0.000 description 14
- 230000005494 condensation Effects 0.000 description 14
- 230000008901 benefit Effects 0.000 description 12
- 239000007789 gas Substances 0.000 description 11
- 238000005259 measurement Methods 0.000 description 11
- 230000000694 effects Effects 0.000 description 10
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 230000008878 coupling Effects 0.000 description 6
- 238000010168 coupling process Methods 0.000 description 6
- 238000005859 coupling reaction Methods 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- RVPVRDXYQKGNMQ-UHFFFAOYSA-N lead(2+) Chemical compound [Pb+2] RVPVRDXYQKGNMQ-UHFFFAOYSA-N 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 230000010287 polarization Effects 0.000 description 4
- 238000007650 screen-printing Methods 0.000 description 4
- 239000005751 Copper oxide Substances 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 3
- 229910000431 copper oxide Inorganic materials 0.000 description 3
- 230000032798 delamination Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000008030 elimination Effects 0.000 description 3
- 238000003379 elimination reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000004907 flux Effects 0.000 description 3
- 238000005247 gettering Methods 0.000 description 3
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 description 3
- 230000005501 phase interface Effects 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 2
- 230000001143 conditioned effect Effects 0.000 description 2
- 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 2
- 239000002003 electrode paste Substances 0.000 description 2
- 229910000464 lead oxide Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 241001676573 Minium Species 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910000978 Pb alloy Inorganic materials 0.000 description 1
- 229910020294 Pb(Zr,Ti)O3 Inorganic materials 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000000254 damaging effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000001939 inductive effect Effects 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
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- XMFOQHDPRMAJNU-UHFFFAOYSA-N lead(II,IV) oxide Inorganic materials O1[Pb]O[Pb]11O[Pb]O1 XMFOQHDPRMAJNU-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 1
- 239000006259 organic additive Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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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
- H10N30/05—Manufacture of multilayered piezoelectric or electrostrictive devices, or parts thereof, e.g. by stacking piezoelectric bodies and electrodes
- H10N30/053—Manufacture of multilayered piezoelectric or electrostrictive devices, or parts thereof, e.g. by stacking piezoelectric bodies and electrodes by integrally sintering piezoelectric or electrostrictive bodies and electrodes
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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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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/638—Removal thereof
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- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/02—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
- C04B37/021—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles in a direct manner, e.g. direct copper bonding [DCB]
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- 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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- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/80—Constructional details
- H10N30/87—Electrodes or interconnections, e.g. leads or terminals
- H10N30/871—Single-layered electrodes of multilayer piezoelectric or electrostrictive devices, e.g. internal electrodes
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- 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
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3281—Copper oxides, cuprates or oxide-forming salts thereof, e.g. CuO or Cu2O
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5445—Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron
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- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
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Definitions
- the present invention relates to a piezoceramic device and a method for manufacturing it wherein the device includes a stack of at least two ceramic layers and an electrode layer arranged between the two ceramic layers.
- Such devices may comprise a plurality of layers and uses. For example, they may be used in: actuators for effecting a low-inertia mechanical vibration of comparably high force via application of a select control voltage; bending elements to effect a high mechanical vibration of less force via application of select control voltage; or production of high electrical voltages. Piezoceramic devices may serve to detect mechanical acoustic vibrations and/or serve in their production via implementation in relevant devicse.
- the electrodes may comprise Ag/Pd in the molar ratio 70/30. At up to several hundred electrode layers, the piezoceramic devices are burdened with substantial costs.
- the precious metal electrodes permit the elimination of thermal dispergers and binders as well as other organic additives used in the process of ceramic foil production.
- organic components of screen printing-metal paste of the multilayer stacks are eliminated via air depolymerisation and oxydation such that a later sinter condensation at approximately 1100° C. to 1150° C. is made possible without damaging effects. Such effects may for example be effected by residual carbon which negatively influences the characteristics of the ceramics due to reduction reactions.
- La 2 O 3 or Nd 2 O 3 doped Pb(Zr,Ti)O 3 ceramics are documentated in the literature, including by G. H. Haertling in the American Ceramic Society Bulletin (43(12), 113-118 (1964) and Journal of the American Ceramic Society 54, 1-11 (1971) as well as in Piezoelectric Ceramics , Academic Press, London and New York (1971) of B. jaffe, W. R. Cook and H. Jaffe. Additional discussion may be found in Y. Xu in Ferroelectric Materials and their Applications , Elsevier Science Publishers, Amsterdam (1991).
- La 2 O 3 in particular Nd 2 O 3 —additives induce the production of cation vacancies in the Pb positions of the crystal structure and at the same time increase the tendency to act as donors, particularly at insufficient oxygen partial pressure, which can lead to a depression of the insulating resistance and a rise in the dielectrcial losses, i.e. the sensitivity of the ceramic towards reduction is increased.
- the additives stabilize the tetragonal phase and the kinetics of the orientation of the domains in the field direction at the polarity, i.e. the electromechanical behavior of the “soft piezoceramic” is influenced positively by such additives.
- All of these ceramics are based on Perovskite mixed crystal phases which, in combination with Ag/Pd internal electrodes, produce a relatively positive behavior for the purpose of a piezostack when the debindering (the removal of the binder or binders) and the sinter condensation is performed.
- Piezoelectrical ceramic masses of the general composition (Pb 1 ⁇ x ⁇ y Sr x Na ⁇ M y ) a [(Nb b Y c Cr d Co e Sb ⁇ ) f Ti g Zr 1 ⁇ f ⁇ g ]O 3 are set out in U.S. Pat. No.
- the publication DE 9700463 discloses the production of green foils for piezoceramic multilayer devices.
- the green foils are based on a piezoceramic powder of the type PZT, to which a stochiometric surplus of a heterovalent rare earth metal (up to a content from 1 to 5 molar-%) and a stochiometric surplus of an additional 1-5 molar-% lead oxyde is added.
- Ag + -ions from the area of Ag/Pd internal electrodes diffuse into the ceramic layers of the multilayer devices such that the heterovalent doping produced cation vacancies are occupied and accordingly result in a filled up Perovskite structure.
- This structure may be: Pb 0,99 Ag 0,01 La 0,01 [Zr 0,30 Ti 0,36 (Ni 1 ⁇ 3 Nb 2 ⁇ 3 ) 0,34 ]O 3 or Pb 0,96 Ag 0,02 Nd 0,02 (Zr 0,54 , Ti 0,46 )O 3 .
- a piezoceramic is produced with a comparatively high Curie temperature for applications of up to 150° C.
- solidity between the Ag/Pd internal electrode (70/30) and the ceramic, as well as growth during the sintering, are positively influenced by building silver into the ceramic.
- U.S. Pat. No. 5,233,260 discusses piezoactuators which are not produced in the tradiational monolithic manner. Rather, the ceramic layers are separately sintered and only then stacked and agglutinated. This production method is costly. Furthermore, these piezoactuators have the disadvantage that the glue used has a negative effect the electrical characteristics.
- DE 19749858 C1 sets out the production of COG with internal electrodes formed of a ceramic mass with the general composition (Ba II 1 ⁇ y Pb y ) 6 ⁇ x Nd 8+2x/3 Ti 18 O 54 +z m-% TiO 2 +pm-% Glas at lower PbO content(0.6 ⁇ x ⁇ 2.1; 0 ⁇ y ⁇ 0.6, 0 ⁇ z ⁇ 5.5 and 3 ⁇ p ⁇ 10).
- a sufficient elimination of the organic components by feeding steam into the nitrogen flux with ⁇ 10 ⁇ 2 Pa oxygen partial pressure at temperatures up to 680° C. and the sinter condensation at 1000° C. is reached by apt glass frit addititives.
- An advantage of the present invention provides an alternative to the expensive Ag/Pd internal electrodes used in the related art. It is a further advantage to provide a substitution which does not oxidize and remains relatively stable during production. It is still a further advantage to provide a method which can be implemented to enable mass production at reasonable engineering effort and expense and with maximally replicable component characteristics.
- the present invention encompasses all piezoceramic devices available in a monolithic multilayer formation, and in particular Perovskit ceramic. Modifications by mixed crystal formation via building in cations on the-A positions and/or substitution of the B-cations with suitable replacement cations or combinations thereof can be effected. Ceramic foil production techniques may be employed along with sintering techniques in the formation of the present invention. For example, screen printing can be used for making the copper or copper mixted internal electrodes.
- Such piezoceramic multilayer devices can be realized for example as actuators by an apt process guide, by which the debindering of the green foil stacks is carried out by steam thereby avoiding the oxidation of the copper containing internal electrodes.
- the following sinter condensation to a monolithic multilayer device can be carried out in an advantageous ways at about 1000° C., i.e. below the melting temperture of the copper.
- a further advantage of the present invention may be found in that for a PZT ceramic mass, copper-containing internal electrodes are applied in place of the normally used Ag/Pd internal electrodes (70/30) on the basis of the multilayer foil technique, whereby the practically complete debindering can be successfully done before effecting the sinter condensation, and under inert conditions, in such a way that a lot of steam is supplied to the inert atmosphere during the debindering thereby permitting only a set oxygen partial pressure, and hence leaving the copper containing internal electrodes relatively intact. Accordingly, by the present method, piezoactuators are created which have the same if not superior quality to those currently available. Likewise, the presence of the copper electrodes do not have any deliterious effects on the piezoactuators.
- a preferred step in the present method includes a step wherein cations are built in on A-positions of the ceramic and at which cations on B-positions are replaced by apt other cations or combinations of cations.
- bivalent metal cations M II may be built on A-positions of the ceramic. These can be selected for example from a group of elements, which contain barium, strontium, calcium, copper and bismuth. Bivalent metal cations M II from a group of elements including scandium, yttrium, lantanum or from group of lanthanides can be considered for the A-positions of the ceramic.
- monovalent cations can be built in on the A-positions of the ceramic, which are selected advantegously and from a group of elements which contains silver, copper, sodium and potassium.
- monovalent cations M II and monovalent cations can be built in on A-positions.
- a preferred embodiment includes the partial substitution of the quadrivalent cations Zr and Ti on the B-positions of the ferroelectrical Perovskite ceramic.
- Still a further advantage includes the composition of the ceramic with the general formula
- the invention includes the realization that the by donors, e.g. a rare earth metal doped piezo ceramic on the basis of PZT, because of the formation of cation vacancies on the A-positions of the Perovskit structure, e.g. according to the composition Pb II 0,97 Nd III 0,02 V′′Pb,0,01( Zr 0,54 Ti 0,46) O 3 (V′′ meaning an empty space), develops a certain affinity to absorb copper from the internal electrodes without destroying them by elimination of equivalent PbO-shares, whereby the latter combination acts as a sinter aid and up to some percentage of PbO is separately added to the ceramic anyway.
- donors e.g. a rare earth metal doped piezo ceramic on the basis of PZT
- V′′ meaning an empty space
- the sinter condensation is supported by the known mobility of the copper ions and leads, by the copper migration, to a solid adhesion between the electrode layer and ceramic such that delaminations can be effectively avoided.
- FIG. 1 depicts temperature control during debindering and sintering
- FIGS. 2 a and 2 b depict a partial cross section of a multilayer stack with alternating sequence of PZT ceramic foils and Cu-internal electrodes;
- FIGS. 3 a and 3 b depict a measuring curve of copper content of piezoceramic layer and a section view of the piezoceramic layer;
- FIG. 4 depicts a diagram of an excursion curve for a polarized PZT-piezoactuator with Cu-internal electrodes
- FIG. 5 depicts a calculation of thermodynamic data as curves for different H 2 /H 2 O concentrations.
- a piezoceramic Perovskite-mixed crystal phase is built according to the following steps: TiO 2 , ZrO 2 (each may be from a mixed precipitation produced precursor (Zr, Ti)O 2 ) and PbCo 3 (e.g. Pb 3 O 4 and dopants like La 2 O 3 or from another oxyde of the rare earth metals) and if necessary an additive of CuO based raw material mixture is set in its composition on the morphotropic phase interface with a PbO-surplus of maximally 5% to support the sinter condensation; for even distribution, the component undergoes a grinding step in diluted suspension and is calcinated after the filtering; and drying occurs at 900 to 950° C.
- the finely ground powder is suspended in a diluted slip with approx. 70 m-% solid substance content by use of a disperger, thus corresponding to approximately 24 vol.-%.
- the optimal dispersing dispergator portion is separately determined in a series of tests, which can be recognized by obtaining a certain viscosity minium.
- approximately 6 m-% of a commercial binder is added to the dispersed suspended solids, which is thermohydrolytically degradable. Accordingly, a diluted polyurethane dispersion has been shown to have advantage effects. It is mixed in a disperse mill and accordingly provided for the process of “foil-pulling” (in particular for the production of a spraying granular apt slip).
- Compact green discoids produced from the granular) or small square multilayer printed boards (“MLP” produced by stacking and laminating 40 to 50 ⁇ m thick green foils without print and with Cu-electrode paste) can be debindered up to a residue carbon content of 300 ppm in a H 2 O-steam containg inert atmosphere at a defined oxygen partial pressure, which fulfills the condition of the coexistency of PbO and in particular Bi 2 O 3 -containing piezoceramic and copper.
- MLP small square multilayer printed boards
- the hydrolytical separation of the binder takes place primarily at a low temperature of 200 ⁇ 50° C. and at a steam partial pressure larger than 200 mbar.
- the oxygen partial pressure is set to a value which is well-tolerated by the copper containing electrodes. This is done by gettering the oxygen from the flow of gas at surfaces of Cu or by adding H 2 .
- the flow of gas avoids damage to the ceramic.
- the electrode layers support the debindering, because preferred paths for a binder transportation is created by them, there is still a considerable debindering time necessary, particularly for the actuators with 160 electrodes (measurements 9,8*9,8* 12,7 mm 3 ).
- the invention enables herewith the production of actuators with more than 100 internal electrodes, which has the advantage of a highly obtainable actuator-excursion.
- Examples for a debindering control are found in table 1 by indicating the residue carbon content of the obtained devices.
- the dew point for steam of both debindering programs lies at 75° C., the partial pressure of the steam corresponds to 405 mbar.
- FIG. 1 shows the temperature control during the debindering and sintering.
- the steam partial pressure supplied with the nitrogen flux corresponding to a dew point of 75° C. is indicated as well.
- the sinter condensation is effected at 1000° C. without creating a reductive degradation of the ceramic.
- the dielectrical and especially the piezoelectrical characteristics of the obtained samples with the measurements of approximately 10.10 mm 2 and 0,7 (in particular 2 mm consistency) are measured after contacting by sputtering of Au-electrodes and compared with the air-debindered (sintered at 1130° C.) samples of the same geometry.
- Table 4 depicts effective piezoelectrical coupling factors of the MLP samples from table 3 for two fundamental vibrations, determined from the measurement of each 3 MLP samples, sintered under the indicated conditions (a), (b), (c) and (d) in table 2, Planar vibration Consistency mode of vibration MLP f S/kHz f p/KHz k eff f S/kHz f p/KHz k eff (a) 158 ⁇ 1 191 ⁇ 2 0.56 ⁇ 0.01 3292 ⁇ 15 3848 ⁇ 79 0.52 ⁇ 0.03 (b) 166 ⁇ 2 198 ⁇ 4 0.54 ⁇ 0.01 2900 ⁇ 78 3197 ⁇ 25 0.42 ⁇ 0.05 (c) 163 ⁇ 1 189 ⁇ 5 0.51 ⁇ 0.04 2830 ⁇ 111 3100 ⁇ 108 0.40 ⁇ 0.02 (d) 154 ⁇ 2 186 ⁇ 2 0.56 ⁇ 0.03 2668 ⁇ 36 3048 ⁇ 47 0.48 ⁇ 0.03
- Electromechanical coupling factors which are in the area of the air-sintered samples are accrued from the produced samples sintered commonly under these conditions with copper.
- the results of an excursion measurement on ceramic samples MLP are listed in table 5.
- the excursion ⁇ h was determined parallely to the polarized direction 3, in which the measuring voltage was set.
- the excursion measurement was carried out by inductive path measuring by setting up an electrical field E with a field strength of 2000 V/mm. Prior to this measurement, the samples were impinged by a field strength of 2000 V/mm in the polarized direction to rule out after-polarity effects and increased hysteresis because of the bedding after the polarity.
- d 33 is a geometrically independent value for the piezoelectrical large signal characteristics of the examined ceramic.
- Table 5 sets out an excursion measurement of square ceramic samples ML: (edge length 1, consistency h) with the composition according table 2 by setting a voltage of 2kV/mm. Electrical measurement voltage U, excursion ⁇ h, and the piezoelectrical constant d 33 are indicated.
- a Cu-screen print paste which has a metal content as high as possible of approx. 75 m-% and is processed with a special high-polymer and is thereby a very viscous binder (which produces at already ⁇ 2 m-%, related to the solid susbstance content, a viscosity as thixotrope as possible, preferably >2000 mPa*s).
- multilayer samples “VS” with up to 20 internal electrodes are produced for sampling purposes.
- piezostacks with 100 to 300 Cu-internal electrodes are built up in a second step and are debindered and sintered under the above mentioned conditions of a defined oxygen partial pressure in the presence of steam.
- the piezoceramic green foils are produced in a consistency, which produces, by considering the linear shrinkage during the sintering of typically 15%, a piezoceramic consistency from 20 to 200 ⁇ mm.
- the Cu-electrodes have a layer consistency from 1 to 3 ⁇ m after the sintering.
- FIG. 2 a and 2 b depict a schematic cross section of a multilayer stack with an alternating sequence of PZT ceramic foils and Cu-internal electrodes in 500 times (FIG. 2 a ) and in 1000 times (FIG. 2 b ) enlargement.
- the green foils produced according to the method of the consistency from 40 to 50 ⁇ m are further processed according to the multilayer ceramic condensators method.
- the printing of the square cut PZT ceramic foils is done mechanically by screen printing technique (400 mesh) with the piezo actuators common electrode design by usage of a commercial Cu-electrode paste.
- the stacking is done such that on every two non-printed foils a printed one follows. 100 piezo actuators in a green condition are received from the block, after laminating, and pressing or sawing.
- the debindering is carried out according to the FIG. 1 shown temperature time diagram in nitrogen stream by adding steam and hydrogen so that there is a target value from 5*10 ⁇ 2 to 2*10 ⁇ 1 Pa for the O 2 partial pressure produced in the area of 500° C. Essentially, lower oxygen partial pressures occur locally during the debindering.
- the ceramic is not subject to the reductive degradation in the temperature area of the debindering, because the equilibrated oxygen partial pressure is lowered as well, conditioned thermodynamically, and the reduction processes are kinetically sufficiently obstructed.
- the green parts of the multilayer piezo actuators still show a residue content of carbon of 300 ppm after the debindering and are afterwards ready to be sintered in the same set atmosphere without causing a reductive degradation which lead to cracking, delamination and eventually to drifting of the internal electrodes because of the production of a low melting Cu/Pb-alloy.
- [0063] is used for setting a certain oxygen partial pressure.
- K D p ⁇ ( O 2 ) 1 2 ⁇ p ⁇ ( H 2 ) p ⁇ ( H 2 ⁇ O )
- thermodynamic data a certain oxygen partial pressure is thereby determined at a given temperature for a defined partial pressure ratio of steam and hydrogen.
- the calculation of the thermodynamic data produces the data depicted in FIG. 5, namely the curves for different H 2 /H 2 O ratios of concentration.
- the gas composition is selected in such a way, that the requested oxygen partial pressure is produced at sinter temperature T Sinter .
- T Sinter sinter temperature
- This condition is for example depicted in FIG. 5.
- the p(O 2 ) runs parallel to the other curves with decreasing temperature.
- the p(O 2 ) value is low for T ⁇ T Sinter , which is still tolerable if needed.
- the gas control curve Cu1 according to table 7 corresponds to this process.
- the equilibrium of Pb/PbO falls short starting at approx. 900° C., conditioned by the narrow thermodynamic window through which metallic lead is produced if there is sufficient kinetic activity.
- FIG. 5 shows the calculated course of the partial pressure for the different ratios of concentration of the gases.
- the sinter profile is as follows: the holding time at maximal temperature lies between 2 and 12 hours.
- the heating up ramp and the cooling down ramp are effected at 5 K/min; and the actuators are slowly heated up at 1 K/min.
- the in steps adjusted set-up of the oxygen partial pressure (FIG. 5) runs in conformity with the temperature curve, which is obtained by an alteration of the forming gas flow meter. Thereby, the steam partial pressure (100 g/h) is constant.
- the obtained ceramic is tightly sintered to >96% and shows mostly homogenous low porosity.
- the sinter grains grow according to the piezoelectrical characteristics with an advantageous medium grain size of 0.8-5 ⁇ m. Intact and crack-free actuators are obtained.
- the sequence of the internal electrodes and PZT ceramic layers is shown in a section in FIGS. 2 a and 2 b .
- the piezo actuators are ground and polished for the finishing and contacted in the area of the exiting internal electrodes according to applications common to Cu-paste and burned-in at 935° C. according to a preset temperature time curve.
- the piezo actuators respond to the electrical measuring after the application of wires by known Bond technology.
- FIG. 4 The diagram of a vibration curve for a polarized PZT-piezoactuator with 160 Cu-internal electrodes is depicted in FIG. 4. A density of 0,123% is produced by a voltage setting of 140,6 Volt at a consistency of 70 ⁇ m of the PZT ceramic layers. The piezoelectrical coefficient in direction to the applied field d 33 is 614,6 10 ⁇ 12 m/V.
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Abstract
The present invention relates to a piezoelectrical device whose electrode layers contain copper. The usage of copper in electrode layers is enabled by a debindering process, which is carried out by steam.
Description
- 1. Field of the Invention
- The present invention relates to a piezoceramic device and a method for manufacturing it wherein the device includes a stack of at least two ceramic layers and an electrode layer arranged between the two ceramic layers.
- Such devices may comprise a plurality of layers and uses. For example, they may be used in: actuators for effecting a low-inertia mechanical vibration of comparably high force via application of a select control voltage; bending elements to effect a high mechanical vibration of less force via application of select control voltage; or production of high electrical voltages. Piezoceramic devices may serve to detect mechanical acoustic vibrations and/or serve in their production via implementation in relevant devicse.
- In the manufacture of piezoceramic devices, technical solutions have up until now been predominantly based on ceramic masses of the Perovskite structure type with the general formula ABO3. Herein, the piezoelectrical characteristics are brought to bear in a ferroelectrical condition. Lead zirconate titanate ceramics Pb(Zr1−xTix)O3=PZT, modified with select additives, have been shown to demonstrate particular advantages. The combination of ceramics and additives is tailored to the so-called morphotropic phase interface of two co-existing ferroelectrical phases: a tetragonal and a rhombodic phase. Between the ceramic layers, produced according to known methods of ceramic foil technology, precious metal internal electrodes are applied by screen printing. The electrodes may comprise Ag/Pd in the
molar ratio 70/30. At up to several hundred electrode layers, the piezoceramic devices are burdened with substantial costs. The precious metal electrodes permit the elimination of thermal dispergers and binders as well as other organic additives used in the process of ceramic foil production. Likewise organic components of screen printing-metal paste of the multilayer stacks are eliminated via air depolymerisation and oxydation such that a later sinter condensation at approximately 1100° C. to 1150° C. is made possible without damaging effects. Such effects may for example be effected by residual carbon which negatively influences the characteristics of the ceramics due to reduction reactions. - 2. Description of the Related Art
- Examples of La2O3 or Nd2O3 doped Pb(Zr,Ti)O3 ceramics are documentated in the literature, including by G. H. Haertling in the American Ceramic Society Bulletin (43(12), 113-118 (1964) and Journal of the American Ceramic Society 54, 1-11 (1971) as well as in Piezoelectric Ceramics, Academic Press, London and New York (1971) of B. jaffe, W. R. Cook and H. Jaffe. Additional discussion may be found in Y. Xu in Ferroelectric Materials and their Applications, Elsevier Science Publishers, Amsterdam (1991).
- La2O3—in particular Nd2O3—additives induce the production of cation vacancies in the Pb positions of the crystal structure and at the same time increase the tendency to act as donors, particularly at insufficient oxygen partial pressure, which can lead to a depression of the insulating resistance and a rise in the dielectrcial losses, i.e. the sensitivity of the ceramic towards reduction is increased. At the same time, the additives stabilize the tetragonal phase and the kinetics of the orientation of the domains in the field direction at the polarity, i.e. the electromechanical behavior of the “soft piezoceramic” is influenced positively by such additives. For an advancement of the sinter condensation and prevention of evaporation losses of PbO in the ceramic, a low PbO surplus at the originally weighed-in composition is generally considered. The relationship between doping level by La2O3, in a Pb(Zr0,47Ti0,53)O3-ceramic (supplied with 3 molar-% PbO surplus) is discussed in the Journal of Electroceramics 2(2), 75-84 (1998) by M. Hammer and M. Hoffmann. In the journal, the sinter behavior and structure formation associated therewith and electro magnetic characteristics (such as coupling factor) and dielectricity constant (such as curie temperature, maximum temperature for ferroelectrical) as well as associated piezoelectrical behavior are all examined.
- Ceramic masses with bismuth oxide in place of lead oxide (for example (Bi0.5Na0.5)TiO3—KNbO3—BiScO3) were also taken into consideration by T. Takenaka and H. Nagata in The Proceedings of the 11th Interational Symposium of Applied Ferroelectrics, Montreux 1998, IEEE 98CH36245, 559-562 (1998). Herein, Pb(TixZr1−x)O3 was combined with BiScO3 and/or BiInO3. All of these ceramics are based on Perovskite mixed crystal phases which, in combination with Ag/Pd internal electrodes, produce a relatively positive behavior for the purpose of a piezostack when the debindering (the removal of the binder or binders) and the sinter condensation is performed.
- Piezoelectrical ceramic masses of the general composition (Pb1−x−∝−ySrxNa∝My)a[(NbbYcCrdCoeSbβ)fTigZr1−f−g]O3 are set out in U.S. Pat. No. 5,648,012 and are distinguished by high electromechanical coupling factors, whereby M is at least a rare earth metal of La, Gd, Nd, Sm and Pr and the parameter areas 0.005≦x≦0.08, 0.002≦y≦0.05, 0.95≦a≦1.105, 0.47≦b≦0.70, 0.02≦c≦0.31, 0.11≦d≦0.42, 0.01≦e≦0.12, 0.02≦f≦0.15, 0.46≦g≦0.52,0≦∝≦0.005,0≦β≦0.13 such that b+c+d+e+β=1.00 are effected.
- The publication DE 9700463 discloses the production of green foils for piezoceramic multilayer devices. The green foils are based on a piezoceramic powder of the type PZT, to which a stochiometric surplus of a heterovalent rare earth metal (up to a content from 1 to 5 molar-%) and a stochiometric surplus of an additional 1-5 molar-% lead oxyde is added. In addition, it is disclosed in above publication that Ag+-ions from the area of Ag/Pd internal electrodes diffuse into the ceramic layers of the multilayer devices such that the heterovalent doping produced cation vacancies are occupied and accordingly result in a filled up Perovskite structure. This structure may be: Pb0,99Ag0,01La0,01[Zr0,30Ti0,36(Ni⅓Nb⅔)0,34]O3 or Pb0,96Ag0,02Nd0,02(Zr0,54, Ti0,46)O3. Herein, a piezoceramic is produced with a comparatively high Curie temperature for applications of up to 150° C. Furthermore, solidity between the Ag/Pd internal electrode (70/30) and the ceramic, as well as growth during the sintering, are positively influenced by building silver into the ceramic.
- U.S. Pat. No. 5,233,260 discusses piezoactuators which are not produced in the tradiational monolithic manner. Rather, the ceramic layers are separately sintered and only then stacked and agglutinated. This production method is costly. Furthermore, these piezoactuators have the disadvantage that the glue used has a negative effect the electrical characteristics.
- Cao et al. in the journalAmerican Ceramic Society 76(12) 3019 (1993) discuss a donor doped ceramic and in particular, a Cu foil laid between pre-made ceramic segments Pb0,988(Nb0,024Zr0,528Ti0,473)O3. The sandwich arrangement is subject to sintering at 1050° C. under vacuum. The composite between the ceramic and Cu internal electrode and the absence of the migrational effects (such as those observed at Ag electrodes on air) are emphasized in the article. However, the disclosed method does not lend itself to the requirements of an efficient production, including foil multilayer technology, and is therefore not appropriate for a mass production.
- Kato et al. teach, inCeramic Transactions Vol. 8, pages 54-68 (1990), of the production of multilayer condensators with Z5U based on ceramics having the general formula (Pba—Cab) (Mg⅓Nb⅔)xTiy(Ni½W½)zO2+a+b (a+b>1, x+y+z=1) with Cu internal electrodes, wherein a copper oxide screen-printing paste is used. Air-debindering is thereby made possible. The carbon formation, which would inevitably come into effect under nitrogen at a well tolerated metallic copper (with oxygen) partial pressure, and afterwards at the sinter condensation, leads to a reductive degradation of the ceramic with Cu/Pb alloying production the eutectic melting point lying at TS=954° C. is thereby avoided. After the debindering, the sinter condensation is then carried out at 1000° C. by additional dosage of hydrogen at an oxygen partial pressure of 10−3 Pa and the copper oxide is accordingly reduced to copper. The process is interference-prone, because of the shrinkage during the reduction from copper oxide to copper and resulting delamination and has up to now not been technologically converted into products.
- DE 19749858 C1 sets out the production of COG with internal electrodes formed of a ceramic mass with the general composition (BaII 1−yPby)6−xNd8+2x/3Ti18O54+z m-% TiO2+pm-% Glas at lower PbO content(0.6<x<2.1; 0<y<0.6, 0<z<5.5 and 3<p<10). A sufficient elimination of the organic components by feeding steam into the nitrogen flux with <10−2 Pa oxygen partial pressure at temperatures up to 680° C. and the sinter condensation at 1000° C. is reached by apt glass frit addititives.
- An advantage of the present invention provides an alternative to the expensive Ag/Pd internal electrodes used in the related art. It is a further advantage to provide a substitution which does not oxidize and remains relatively stable during production. It is still a further advantage to provide a method which can be implemented to enable mass production at reasonable engineering effort and expense and with maximally replicable component characteristics. These and other advantages are realized by the present invention wherein, copper is substituted for Ag/Pd for use in a PZT-type piezoceramic multilayer element. Copper has been shown not to reduce or oxidize and otherwise remain stable under conditions, including temperatures around 1000° C. under low oxygen partial pressure of <10−2.
- The present invention encompasses all piezoceramic devices available in a monolithic multilayer formation, and in particular Perovskit ceramic. Modifications by mixed crystal formation via building in cations on the-A positions and/or substitution of the B-cations with suitable replacement cations or combinations thereof can be effected. Ceramic foil production techniques may be employed along with sintering techniques in the formation of the present invention. For example, screen printing can be used for making the copper or copper mixted internal electrodes.
- Such piezoceramic multilayer devices can be realized for example as actuators by an apt process guide, by which the debindering of the green foil stacks is carried out by steam thereby avoiding the oxidation of the copper containing internal electrodes. The following sinter condensation to a monolithic multilayer device can be carried out in an advantageous ways at about 1000° C., i.e. below the melting temperture of the copper. A further advantage of the present invention may be found in that for a PZT ceramic mass, copper-containing internal electrodes are applied in place of the normally used Ag/Pd internal electrodes (70/30) on the basis of the multilayer foil technique, whereby the practically complete debindering can be successfully done before effecting the sinter condensation, and under inert conditions, in such a way that a lot of steam is supplied to the inert atmosphere during the debindering thereby permitting only a set oxygen partial pressure, and hence leaving the copper containing internal electrodes relatively intact. Accordingly, by the present method, piezoactuators are created which have the same if not superior quality to those currently available. Likewise, the presence of the copper electrodes do not have any deliterious effects on the piezoactuators.
- A preferred step in the present method includes a step wherein cations are built in on A-positions of the ceramic and at which cations on B-positions are replaced by apt other cations or combinations of cations. For example, on A-positions of the ceramic bivalent metal cations MII may be built. These can be selected for example from a group of elements, which contain barium, strontium, calcium, copper and bismuth. Bivalent metal cations MII from a group of elements including scandium, yttrium, lantanum or from group of lanthanides can be considered for the A-positions of the ceramic.
- Further, monovalent cations can be built in on the A-positions of the ceramic, which are selected advantegously and from a group of elements which contains silver, copper, sodium and potassium. In addition it is also possible, to build in combinations of bivalent metal cations MII and monovalent cations on A-positions.
- Furthermore, a preferred embodiment includes the partial substitution of the quadrivalent cations Zr and Ti on the B-positions of the ferroelectrical Perovskite ceramic. In fact, combinations of mono- and quintvalent metal cations MI ¼MV ¾ with MI=Na, K and MV=Nb, Ta or two- and quintvalent metal cations MII ⅓MV ⅔ with MII=Mg, Zn, Ni, Co and MV=Nb, Ta or three- and quintvalent metal cations MIII ½MV ⅔ with MIII=Fe, In, Sc, heavier lanthanide-elements and MV=Nb, Ta or combinations MIII ⅔MVI⅓ with MIII=Fe, In, Sc, heavier lanthanide-elements and MVI=W resp. MII ½MVi ½ with MII=Mg, Co, Ni and MVI=W may be employed.
- Still a further advantage includes the composition of the ceramic with the general formula
-
z Ti0,46+z)O3 wherein 0,01<x<0,05,−0,15<z<+0,15 and 0<y<0,06, whereby SE is a rare earth metal, V is a vacancy and a PbO-surplus is set from 1 up to maximally 5 molar-%. - Yet further, atop the ceramic an additive of CuO may be included.
- The invention includes the realization that the by donors, e.g. a rare earth metal doped piezo ceramic on the basis of PZT, because of the formation of cation vacancies on the A-positions of the Perovskit structure, e.g. according to the composition PbII 0,97 NdIII 0,02 V″Pb,0,01(Zr0,54Ti0,46)O3 (V″ meaning an empty space), develops a certain affinity to absorb copper from the internal electrodes without destroying them by elimination of equivalent PbO-shares, whereby the latter combination acts as a sinter aid and up to some percentage of PbO is separately added to the ceramic anyway.
- The sinter condensation is supported by the known mobility of the copper ions and leads, by the copper migration, to a solid adhesion between the electrode layer and ceramic such that delaminations can be effectively avoided.
- It is still further an advantage to already add some CuO within the
limits 0<y<0,15 to the original mixture of the used recipe for piezostacks, e.g. on the basis of PZT with Cu-internal electrodes corresponding to the general formula PbII 1−x−ySEIII xCuyV″x/2(Zr 0,54−zTi0,46+z)O3 with 0,005<x<0,05 and −0,15<z<+0,15 (SE=Rare Earth Metal). The piezoelectrical characteristics, like the high value for the electromechanical coupling factor can be maintained at corresponding adjustment of the parameter z to the morphotropic phase interface. - Some of the features, advantages, and benefits of the present invention having been stated, others will become apparent as the description proceeds when taken in conjunction with the accompanying drawings wherein:
- FIG. 1 depicts temperature control during debindering and sintering;
- FIGS. 2a and 2 b depict a partial cross section of a multilayer stack with alternating sequence of PZT ceramic foils and Cu-internal electrodes;
- FIGS. 3a and 3 b depict a measuring curve of copper content of piezoceramic layer and a section view of the piezoceramic layer;
- FIG. 4 depicts a diagram of an excursion curve for a polarized PZT-piezoactuator with Cu-internal electrodes; and
- FIG. 5 depicts a calculation of thermodynamic data as curves for different H2/H2O concentrations.
- A piezoceramic Perovskite-mixed crystal phase is built according to the following steps: TiO2, ZrO2 (each may be from a mixed precipitation produced precursor (Zr, Ti)O2) and PbCo3 (e.g. Pb3O4 and dopants like La2O3 or from another oxyde of the rare earth metals) and if necessary an additive of CuO based raw material mixture is set in its composition on the morphotropic phase interface with a PbO-surplus of maximally 5% to support the sinter condensation; for even distribution, the component undergoes a grinding step in diluted suspension and is calcinated after the filtering; and drying occurs at 900 to 950° C. To obtain sinter condensation in 2 to 4 hours at about 1000° below the melting temperature of copper, a pulverization to a medium grain size <0,4 μm is necessary. The sinter activity of the powder is normally sufficient to guarantee a condensation of >96% of the theoretical density at both sufficient grain growth and adequate mechanical solidity in the ceramic structure.
- The finely ground powder is suspended in a diluted slip with approx. 70 m-% solid substance content by use of a disperger, thus corresponding to approximately 24 vol.-%. For this, the optimal dispersing dispergator portion is separately determined in a series of tests, which can be recognized by obtaining a certain viscosity minium. For the formation of the piezoceramic-green foils, approximately 6 m-% of a commercial binder is added to the dispersed suspended solids, which is thermohydrolytically degradable. Accordingly, a diluted polyurethane dispersion has been shown to have advantage effects. It is mixed in a disperse mill and accordingly provided for the process of “foil-pulling” (in particular for the production of a spraying granular apt slip).
- Compact green discoids (produced from the granular) or small square multilayer printed boards (“MLP” produced by stacking and laminating 40 to 50 μm thick green foils without print and with Cu-electrode paste) can be debindered up to a residue carbon content of 300 ppm in a H2O-steam containg inert atmosphere at a defined oxygen partial pressure, which fulfills the condition of the coexistency of PbO and in particular Bi2O3-containing piezoceramic and copper.
- The hydrolytical separation of the binder takes place primarily at a low temperature of 200±50° C. and at a steam partial pressure larger than 200 mbar. The oxygen partial pressure is set to a value which is well-tolerated by the copper containing electrodes. This is done by gettering the oxygen from the flow of gas at surfaces of Cu or by adding H2. During the debindering by oxidation, the flow of gas avoids damage to the ceramic. Although the electrode layers support the debindering, because preferred paths for a binder transportation is created by them, there is still a considerable debindering time necessary, particularly for the actuators with 160 electrodes (measurements 9,8*9,8* 12,7 mm3).
- The invention enables herewith the production of actuators with more than 100 internal electrodes, which has the advantage of a highly obtainable actuator-excursion. Examples for a debindering control are found in table 1 by indicating the residue carbon content of the obtained devices. The dew point for steam of both debindering programs lies at 75° C., the partial pressure of the steam corresponds to 405 mbar.
TABLE 1 Debindering of ceramic samples MLP and actuators Profile Conditions (R: ramp, H: holding time) Samples C EK 1 R: 30 K/h H: 220° C./10 h R: 30 K/h Ceramic 240 H: 500° C./20 h, at 100 l/h N2, 30 g/h samples H2O, with Cu-gettering MLP EK 2 R: 30 K/h H: 220° C./40 h R: 30 K/h Actuator 160 300 ± H: 500° C./20 h, at 100 l/h N2, 30 g/h electrodes 30 H2O, with Cu-gettering - The soaking time at 220° C. is prolonged to 40 h for actuators with 160 layers (EK 2). Afterwards a condensation of the ceramic at 1000° C. without detrimental reductive degradation is effected with the residue carbon of 300±30 ppm in the indicated sinter profile.
- FIG. 1 shows the temperature control during the debindering and sintering. The steam partial pressure supplied with the nitrogen flux corresponding to a dew point of 75° C. is indicated as well. At such debindered PZT-ceramic samples, the sinter condensation is effected at 1000° C. without creating a reductive degradation of the ceramic. The dielectrical and especially the piezoelectrical characteristics of the obtained samples with the measurements of approximately 10.10 mm2 and 0,7 (in particular 2 mm consistency) are measured after contacting by sputtering of Au-electrodes and compared with the air-debindered (sintered at 1130° C.) samples of the same geometry.
- For air-sinterings of ceramic samples MLP without internal electrodes with the composition PbII 0,97NdIII 0,02V′″0,01(Zr0,54 Ti0,46)O3 and under inert conditions, whereby the latter correspond to the requirements of a common sintering with copper, the results of the electrical measurings are compiled in table 2. Measurements of the polarized samples are set out in tables 3 to 5. In addition, the codes of a CuO-doped ceramic mass during sintering under inert conditions are also set out.
- Table 2 includes characteristics of square ceramic samples MLP (
edge length 1, consistency h): Samples (a), (b) and (c) with composition Pb0,97Nd0,02(Zr0,54Ti0,46)O3. Sample (d) with the composition Pb0,96Cu0,02Nd0,02(Zr0,54Ti0,46)O3 (a) powder pre-ground to a medium grain size d50%=0,53 μm, air-sintering at 1120 °C.; (b), (c) and (d) powder finely ground to a medium grain size d50%=0,33 μm, air-sintered (b) at 1000 °C. resp. (c) and (d) at 1000 °C. under N2/H2O-steam are also set out.Sample MLP h/ mm 1/mm C/nF ε Tan δ RIS/Ω ρ/Ωcm (a) 0.59 ± 0.02 10.8 ± 0.1 2.20 ± 0.05 1268 ± 30 2.1 ± 0.1% 1 * 2 * 1011 1012 (b) 0.70 ± 0.01 10.6 ± 0.1 1.60 ± 0.03 1137 ± 58 2.8 ± 0.2% 2 * 3 * 1011 1012 (c) 0.71 ± 0.02 11.0 ± 0.8 1.62 ± 0.07 1132 ± 81 2.8 ± 0.6% 5 * 9 * 109 1010 (d) 0.70 ± 0.01 11.3 ± 0.1 1.92 ± 0.01 1196 ± 8 1.9 ± 0.3% 7 * 1 * 1010 1212 -
TABLE 3 Characteristics of square ceramic samples MLP ( edge length 1,consistency h) with the composition according to table 2 after the polarity with 1200 V (a) and 1400 V ((b) and (c) and (d)). Sample MLP h/ mm 1/mm C/nF ε Tan δ□ RIS/Ω ρ/Ωcm (a) 0.59 ± 0.02 10.8 ± 0.1 2.54 ± 0.13 1460 ± 134 1.9 ± 0.1% 1 * 2 * 1011 1012 (b) 0.70 ± 0.01 10.6 ± 0.1 1.70 ± 0.03 1207 ± 58 2.1 ± 0.1% * 2 * 1011 1012 (c) 0.71 ± 0.02 11.0 ± 0.8 1.75 ± 0.05 1238 ± 69 2.3 ± 0.1% 2 * 5 1011 1012 (d) 0.70 ± 0.01 11.3 ± 0.1 2.11 ± 0.01 1317 ± 69 10.2 ± 0.8% 8 * 1 * 1010 1012 - The characteristic values prove that PZT ceramic samples, which were not air-bindered and were sintered, show comparable dielectrical characteristics.
-
-
- As such, the proportion of the mechanical energy for the entire energy is indicated by C1/(C0+C1).
- Table 4 depicts effective piezoelectrical coupling factors of the MLP samples from table 3 for two fundamental vibrations, determined from the measurement of each 3 MLP samples, sintered under the indicated conditions (a), (b), (c) and (d) in table 2,
Planar vibration Consistency mode of vibration MLP fS/kHz fp/KHz keff fS/kHz fp/KHz keff (a) 158 ± 1 191 ± 2 0.56 ± 0.01 3292 ± 15 3848 ± 79 0.52 ± 0.03 (b) 166 ± 2 198 ± 4 0.54 ± 0.01 2900 ± 78 3197 ± 25 0.42 ± 0.05 (c) 163 ± 1 189 ± 5 0.51 ± 0.04 2830 ± 111 3100 ± 108 0.40 ± 0.02 (d) 154 ± 2 186 ± 2 0.56 ± 0.03 2668 ± 36 3048 ± 47 0.48 ± 0.03 - The measurement of the Curie temperature at samples (c) show a value of 339±2° C.
- Electromechanical coupling factors which are in the area of the air-sintered samples are accrued from the produced samples sintered commonly under these conditions with copper. The results of an excursion measurement on ceramic samples MLP are listed in table 5. The excursion Δh was determined parallely to the polarized direction 3, in which the measuring voltage was set. The excursion measurement was carried out by inductive path measuring by setting up an electrical field E with a field strength of 2000 V/mm. Prior to this measurement, the samples were impinged by a field strength of 2000 V/mm in the polarized direction to rule out after-polarity effects and increased hysteresis because of the bedding after the polarity.
- The relative density S of the ceramic samples MLP is calculated from the measured excursion Δh divided by the sample consistency h. From this, the piezoelectrical coefficient d33 results for the equation:
- S 3 =d 33 *E 3
- wherein d33 is a geometrically independent value for the piezoelectrical large signal characteristics of the examined ceramic.
- Table 5 sets out an excursion measurement of square ceramic samples ML: (edge
length 1, consistency h) with the composition according table 2 by setting a voltage of 2kV/mm. Electrical measurement voltage U, excursion Δh, and the piezoelectrical constant d33 are indicated.Sample MLP h/mm U/V Δh/μm d33 · 10−12 m/V (a) 0.59 ± 0.02 1180 ± 4 0.88 ± 0.01 747 ± 10 (b) 0.70 ± 0.01 1400 ± 4 0.99 ± 0.01 712 ± 10 (c) 0.71 ± 0.02 1420 ± 4 1.03 ± 0.06 723 ± 40 (d) 0.70 ± 0.01 1400 ± 4 1.03 ± 0.01 739 ± 4 - In case of printing on Cu-internal electrodes, a Cu-screen print paste is preferable which has a metal content as high as possible of approx. 75 m-% and is processed with a special high-polymer and is thereby a very viscous binder (which produces at already <2 m-%, related to the solid susbstance content, a viscosity as thixotrope as possible, preferably >2000 mPa*s). First, multilayer samples “VS” with up to 20 internal electrodes are produced for sampling purposes. Thereafter, piezostacks with 100 to 300 Cu-internal electrodes are built up in a second step and are debindered and sintered under the above mentioned conditions of a defined oxygen partial pressure in the presence of steam.
- The piezoceramic green foils are produced in a consistency, which produces, by considering the linear shrinkage during the sintering of typically 15%, a piezoceramic consistency from 20 to 200 μmm. The Cu-electrodes have a layer consistency from 1 to 3 μm after the sintering.
- FIG. 2a and 2 b depict a schematic cross section of a multilayer stack with an alternating sequence of PZT ceramic foils and Cu-internal electrodes in 500 times (FIG. 2a) and in 1000 times (FIG. 2b) enlargement.
- FIG. 3b shows a measuring curve for the Cu-content of the piezoceramic layer, shown in FIG. 3a, about the layer consistency after the sintering of a piezostack on the basis of the used original composition PbII 0,97−yNd0,02CuyV″0,01(Zr0,54−zTi0,46+z)O3. It can be seen that the copper content in the ceramic layer dissolves starting from the border. The calibration produces in the middle of the ceramic layer the minimal amount of y=0.001. At the borders there is a value which is 20 times higher. Some lead oxide is displaced from the combination as a result of the influence of diffused Cu-ions. The good connection of the Cu-internal electrodes to the ceramic is thereby set out.
- The electrical characteristics of the multilayer ceramic components VS of the original composition Pb0,97Nd0,02V0,01(Zr0,54Ti0,46)O3 after the sintering at 1000° C. with 16 Cu-internal electrodes—and for comparison with 20 Ag/Pd-internal electrodes (70/30) after the air-sintering at 1120° C.—are indicated in table 6. Table 6 sets out electrical characteristics of PZT multilayer ceramic samples VS on the basis of the original composition
- PbII 0,97NdIII 0,02V″0,01(Zr0,54Ti0,46)O3: (a) powder pre-ground, medium grain size d50%=0,53 μm, 20 internal electrodes Ag/Pd (70/30), air-sintering at 1120° C., (c) powder finely ground, medium particle size d50%=0,33 μm, 16 Cu-internal electrodes, sintering at 1000° C. under inert conditions by N2/H2O steam.
ε ε tan δ ρIS/Ωcm Sample before after after after VS Comments C/nF polarization polarization polarization polarization (a) Ag/Pd (70/30): 125 ± 5 1104 ± 54 1561 ± 92 0.015 7.9 1011 Debindering/air-sintering 1120° C., Cu-finished. (c1) Cu-internal electrodes: 110 ± 4 908 ± 35 953 ± 37 0.027 2.7 1010 Debindering/sintering under N2/H2O steam, Cu-finished. (c2) Cu-internal electrodes: 114 ± 4 946 1013 0.026 1.6 1010 Debindering/sintering under N2, H2O steam, Cu-finished. - Production of a piezo actuator from a ceramic of PZT type with Cu-internal electrodes.
- For the production of piezo actuators with 160 Cu-internal electrodes, the green foils produced according to the method of the consistency from 40 to 50 μm are further processed according to the multilayer ceramic condensators method. The printing of the square cut PZT ceramic foils is done mechanically by screen printing technique (400 mesh) with the piezo actuators common electrode design by usage of a commercial Cu-electrode paste. The stacking is done such that on every two non-printed foils a printed one follows. 100 piezo actuators in a green condition are received from the block, after laminating, and pressing or sawing.
- The debindering is carried out according to the FIG. 1 shown temperature time diagram in nitrogen stream by adding steam and hydrogen so that there is a target value from 5*10−2 to 2*10−1 Pa for the O2 partial pressure produced in the area of 500° C. Essentially, lower oxygen partial pressures occur locally during the debindering. The ceramic is not subject to the reductive degradation in the temperature area of the debindering, because the equilibrated oxygen partial pressure is lowered as well, conditioned thermodynamically, and the reduction processes are kinetically sufficiently obstructed. The green parts of the multilayer piezo actuators still show a residue content of carbon of 300 ppm after the debindering and are afterwards ready to be sintered in the same set atmosphere without causing a reductive degradation which lead to cracking, delamination and eventually to drifting of the internal electrodes because of the production of a low melting Cu/Pb-alloy.
-
-
- a certain oxygen partial pressure is thereby determined at a given temperature for a defined partial pressure ratio of steam and hydrogen. The calculation of the thermodynamic data produces the data depicted in FIG. 5, namely the curves for different H2/H2O ratios of concentration.
- Normally the gas composition is selected in such a way, that the requested oxygen partial pressure is produced at sinter temperature TSinter. This condition is for example depicted in FIG. 5. Starting from this value the p(O2) runs parallel to the other curves with decreasing temperature. However, the p(O2) value is low for T<TSinter, which is still tolerable if needed. The gas control curve Cu1 according to table 7 corresponds to this process. The equilibrium of Pb/PbO falls short starting at approx. 900° C., conditioned by the narrow thermodynamic window through which metallic lead is produced if there is sufficient kinetic activity.
- Alternatively, p(O2) was set with different forming gas dosage corresponding to the gas control Cu2—the actual course of the oxygen partial pressure at upto 400° C. lay in the thermodynamic window. This way of process is good for the little reductive solid PZT mixture. The used adjustments Cu1 and Cu2 for the gas control are indicated in table 7. FIG. 5 shows the calculated course of the partial pressure for the different ratios of concentration of the gases.
TABLE 7 Gas control Cu1 and Cu2 Cu1 Dosage Cu2 Dosage N2 Entire sintering 900 l/h Entire sintering 1200 l/h H2/H2O Entire sintering 40 g/h Entire sintering 100 g/h N2 + 5% H2 Entrie sintering 256 ml/h 25-650° C. 25 ml/h 650-900° C. 85 ml/h 900-1000° C. 200 ml/h Dewing point Dewing point 36° C. 48° C. - The sinter profile is as follows: the holding time at maximal temperature lies between 2 and 12 hours. The heating up ramp and the cooling down ramp are effected at 5 K/min; and the actuators are slowly heated up at 1 K/min. The in steps adjusted set-up of the oxygen partial pressure (FIG. 5) runs in conformity with the temperature curve, which is obtained by an alteration of the forming gas flow meter. Thereby, the steam partial pressure (100 g/h) is constant.
- The obtained ceramic is tightly sintered to >96% and shows mostly homogenous low porosity. The sinter grains grow according to the piezoelectrical characteristics with an advantageous medium grain size of 0.8-5 μm. Intact and crack-free actuators are obtained. The sequence of the internal electrodes and PZT ceramic layers is shown in a section in FIGS. 2a and 2 b. The medium grain size in the ceramic structure is d50=1,6±0,3 μm.
- The piezo actuators are ground and polished for the finishing and contacted in the area of the exiting internal electrodes according to applications common to Cu-paste and burned-in at 935° C. according to a preset temperature time curve. The piezo actuators respond to the electrical measuring after the application of wires by known Bond technology.
- The diagram of a vibration curve for a polarized PZT-piezoactuator with 160 Cu-internal electrodes is depicted in FIG. 4. A density of 0,123% is produced by a voltage setting of 140,6 Volt at a consistency of 70 μm of the PZT ceramic layers. The piezoelectrical coefficient in direction to the applied field d33 is 614,6 10−12 m/V.
- The invention being thus described, it will be obvious that the same may be varied in many ways. Such variations are not to be regarded as a departure from the spirit and scope of the invention, and all such modifications as would be obvious to one skilled in the art are intended to be included within the scope of the following claims.
Claims (44)
1. A piezoelectric device comprising a monolithic multilayer form with a stack of at least two ceramic layers and an electrode layer set in between said two ceramic layers wherein said electrode layer contains copper.
2. The device according to claim 1 , wherein said multilayer form is produced from ceramic green foils which contain a thermohydrolithically degradable binder.
3. The device according to claim 2 , wherein said binder is a polyurethane dispersion.
4. The device according to one of the claim 1 , wherein the density of said ceramic layers is at least 96% of said ceramic layers theoretically obtainable density.
5. The device according to one of the claim 2 , wherein the density of said ceramic layers shows at least 96% of said theoretically obtainable density.
6. The device according to claim 1 , wherein said ceramic layers contain grains having a grain size in a range between and including 0,8 and 5 μm.
7. The device according to claim 2 , wherein said ceramic layers contain grains having a grain size in a range between and including 0,8 and 5 μm.
8. The device according to claim 4 , wherein said ceramic layers contain grains having a grain size in a range between and including 0,8 and 5 μm.
9. The device according to claim 1 , wherein said device includes at least 10 stacked electrode layers.
10. The device according to claim 2 , wherein said device includes at least 10 stacked electrode layers.
11. The device according to claim 4 , wherein said device includes at least 10 stacked electrode layers.
12. The device according to claim 6 , wherein said device includes at least 10 stacked electrode layers.
13. The device according to claim 1 , wherein said ceramic layers contain a ferroelectrical Perovskite-ceramic having a general composition ABO3.
14. The device according to claim 2 , wherein said ceramic layers contain a ferroelectrical Perovskite-ceramic having a general composition ABO3.
15. The device according to claim 4 , wherein said ceramic layers contain a ferroelectrical Perovskite-ceramic having a general composition ABO3.
16. The device according to claim 6 , wherein said ceramic layers contain a ferroelectrical Perovskite-ceramic having a general composition ABO3.
17. The device according to claim 9 , wherein said ceramic layers contain a ferroelectrical Perovskite-ceramic having a general composition ABO3.
18. The device according to claim 13 , wherein said Perovskite-ceramic is of a PZT type Pb(ZrxTi1−x)O3.
19. The device according to claim 13 , wherein cations are built on A-positions of the ceramic and where cations on B-positions are replaced by apt other cations or combinations of cations.
20. The device according to claim 18 , wherein cations are built on A-positions of the ceramic and where cations on B-positions are replaced by apt other cations or combinations of cations.
21. The device according to claim 19 , wherein bivalent metal cations MII are built in on A-positions of the ceramic.
22. The device according to claim 21 , wherein said bivalent metal cations MII are selected from a group comprising barium, strontium, calcium and copper.
23. The device according to claim 21 , wherein partially trivalent metal cations MIII are built on A-positions of said ceramic, said metal cations MIII selected from a group comprising scandium, yttrium, bismuth and lanthanum.
24. The device according to claim 21 , wherein partially trivalent metal cations MIII are built on said A-positions of the ceramic, said metal cations MIII being selected from a group comprising lanthanides.
25. The device according to claim 21 , wherein monovalent cations are integrated on A-positions of said ceramic.
26. The device according to claim 25 , wherein said monovalent cations are selected from a group comprising silver, copper, sodium and potassium.
27. The device according to claim 21 , wherein combinations of bivalent metal cations MII and monovalent cations are integrated on A-positions of said ceramic.
28. The device according to claim 25 , wherein combinations of bivalent metal cations MII and monovalent cations are integrated on A-positions of said ceramic.
29. The device according to claim 17 , wherein for partial substitution of quadrivalent cations Zr and Ti on B-positions of said Perovskite ceramic, combinations of at least two of mono- and quinvalent metal cations MI1/4MV3/4 with MI=Na, K and MV=Nb, Ta are used.
30. The device according to claim 17 , wherein for partial substitution of quadrivalent cations Zr and Ti on B-positions of said Perovskite ceramic, at least one of bi- and quintvalent metal cations MII1/3MV2/3 with MII=Mg, Zn, Ni, Co and MV=Nb, Ta are used.
31. The device according to claim 17 , wherein for partial substitution of quadrivalent cations Zr and Ti on B-positions of said ferroelectrical Perovskite ceramic, at least one of tri- and quintvalent metal cations MIII1/2MV2/3 with MIII=Fe, In, Sc, heavier lanthanide elements and MV=Nb, Ta are used.
32. The device according to claim 17 , wherein for partial substitution of quadrivalent cations Zr and Ti on B-positions of said ferroelectrical Perovskite ceramic, combinations of at least two of MIII2/3 MVI1/3 with MIII=Fe, In, Sc, heavier lanthanide elements and MVI=W are used.
33. The device according to claim 17 , wherein for partial substitution of quadrivalent cations Zr and Ti on the B-positions of ferroelectrical Perovskite ceramic, combinations of MII1/2MVI1/2 with MII=Mg, Co, Ni and MVI=W are used.
34. The device according to claim 20 , said ceramic comprises Pb1−x−ySExCuyV′″X/2(Zr0,54−zTi0,46+z)O3 wherein 0,01<x<0,05,−0,15<z,+0,15,0<y<0,06, SE is a rare earth metal, V is a vacancy and a PbO surplus from 1 to maximally 5 molar-% is employed.
35. The device according to claim 20 , wherein said ceramic includes an additive of CuO.
36. A method for producing a piezoelectric device, comprising the steps of:
producting a stack of ceramic green foil comprising binder and electrode layers formed by stacking and laminating green foils; and
debindering said stack of ceramic green foils in an atmosphere comprising an inert gas and oxygen, whereby the oxygen content is reduced by adding an apt amount of hydrogen such that said electrode layers are not damaged.
37. The method according to claim 36 , wherein said step of debindering is carried out at a temperature in a range between and including 150 to 600° C.
38. The method according to claim 36 , wherein said atmosphere includes hydrogen with a partial pressure of upto and including 200 mbar.
39. The method according to claim 37 , wherein said atmosphere includes hydrogen with a partial pressure of upto and including 200 mbar.
40. The method according to claim 36 further comprising the step of sintering said stack at a temperature which is below melting point of copper, said sintering occuring in an atmosphere comprising nitrogen, hydrogen and steam, and wherein oxygen partial pressure is set by an apt hydrogen concentration such that equilibrate partial pressure of equilibrium Cu/CU2O is not exceeded.
41. The method according to claim 37 further comprising the step of sintering said stack at a temperature which is below melting point of copper, said sintering occuring in an atmosphere comprising nitrogen, hydrogen and steam, and wherein oxygen partial pressure is set by an apt hydrogen concentration such that equilibrate partial pressure of equilibrium Cu/Cu2O is not exceeded.
42. The method according to claim 38 further comprising the step of sintering said stack at a temperature which is below melting point of copper, said sintering occuring in an atmosphere comprising nitrogen, hydrogen and steam, and wherein oxygen partial pressure is set by an apt hydrogen concentration such that equilibrate partial pressure of equilibrium Cu/Cu2O is not exceeded.
43. Method according to claim 37 , wherein said temperature is maintained for a duration of 2 to 12 hours.
44. A method for producing a piezoelectric device, comprising the steps of:
first producting a stack of a ceramic green foil comprising binder and electrode layers by stacking and laminating green foils;
second debindering said stack in an atmosphere comprising an inert gas and oxygen, whereby oxygen content is reduced by adding an apt amount of hydrogen such that said electrode layers are not damaged; and
sintering said stack at a temperature which is below melting point of copper, said sintering occuring in an atmosphere comprising nitrogen, hydrogen and steam, and wherein oxygen partial pressure is set by an apt hydrogen concentration such that equilibrate partial pressure of equilibrium Cu/Cu2O is not exceeded.
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Also Published As
Publication number | Publication date |
---|---|
US20100294419A1 (en) | 2010-11-25 |
AU2830701A (en) | 2001-06-25 |
CN1409876A (en) | 2003-04-09 |
WO2001045138A3 (en) | 2002-03-14 |
DE50015994D1 (en) | 2010-10-28 |
ATE481743T1 (en) | 2010-10-15 |
US8209828B2 (en) | 2012-07-03 |
BR0016390A (en) | 2002-08-20 |
EP1240675A2 (en) | 2002-09-18 |
DE10062672B4 (en) | 2010-01-21 |
DE10062672B9 (en) | 2012-07-12 |
DE10062672A1 (en) | 2001-08-02 |
WO2001045138A2 (en) | 2001-06-21 |
JP2003529917A (en) | 2003-10-07 |
EP1240675B1 (en) | 2010-09-15 |
DE20023051U1 (en) | 2003-01-09 |
JP4248581B2 (en) | 2009-04-02 |
EP2278634A3 (en) | 2012-09-05 |
US7855488B2 (en) | 2010-12-21 |
US20060251911A1 (en) | 2006-11-09 |
JP4744052B2 (en) | 2011-08-10 |
JP2007150350A (en) | 2007-06-14 |
EP2278634A2 (en) | 2011-01-26 |
CN1246914C (en) | 2006-03-22 |
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