# US 10,483,454 B2 · Piezoelectric component and method for producing a piezoelectric component

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- Number: US 10,483,454 B2
- Document ID: US10483454B2
- Status: Granted
- Kind: B2
- Application number: 15/361,436
- Filed: 2016-11-27
- Published: 2017-05-18
- Granted: 2019-11-19
- Earliest claimed: 2011-08-30
- Assignees: TDK Electronics Co., Ltd.
- Applicants: TDK Electronics AG
- Inventors: Alexander Glazunov; Adalbert Feltz
- Web page: https://patentgrep.com/patent/US10483454B2

## CPC

- H10N 30/053: by integrally sintering piezoelectric or electrostrictive bodies and electrodes
- C04B 35/491: based on lead zirconates and lead titanates {, e.g. PZT}
- C04B 35/493: containing also other lead compounds
- C04B 35/62222: {obtaining ceramic coatings (coating of mortars, concrete, artificial or natural stone or ceramics C04B41/45; laminated ceramic products B32B18/00; coating of glass C03C17/00, applying ceramic coatings on silicon for semi-conductor purposes H10W; coating metallic materials C23)}
- C04B 35/6261: {Milling}
- C04B 35/6262: {of calcined, sintered clinker or ceramics}
- C04B 35/62645: {Thermal treatment of powders or mixtures thereof other than sintering}
- C04B 35/62685: {characterised by the order of addition of constituents or additives}
- C04B 35/6303: {Inorganic additives}
- C04B 35/638: Removal thereof
- C04B 35/64: Burning or sintering processes (C04B33/32 takes precedence {; powder metallurgy B22F})
- C04B 41/009: {characterised by the material treated}
- C04B 41/5111: {Ag, Au, Pd, Pt or Cu}
- C04B 41/88: Metals
- H10N 30/853: Ceramic compositions
- H10N 30/8554: {Lead-zirconium titanate [PZT] based}
- H10N 30/871: {Single-layered electrodes of multilayer piezoelectric or electrostrictive devices, e.g. internal electrodes}
- H10N 30/877: {Conductive materials}
- C04B 2235/3213: Strontium oxides or oxide-forming salts thereof
- C04B 2235/3215: Barium oxides or oxide-forming salts thereof
- C04B 2235/3224: Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B 2235/3225: Yttrium oxide or oxide-forming salts thereof
- C04B 2235/3236: Alkaline earth titanates
- C04B 2235/3239: Vanadium oxides, vanadates or oxide forming salts thereof, e.g. magnesium vanadate
- C04B 2235/3249: containing also titanium oxide or titanates, e.g. lead zirconate titanate (PZT)
- C04B 2235/3258: Tungsten oxides, tungstates, or oxide-forming salts thereof
- C04B 2235/3281: Copper oxides, cuprates or oxide-forming salts thereof, e.g. CuO or Cu2O
- C04B 2235/3296: Lead oxides, plumbates or oxide forming salts thereof, e.g. silver plumbate
- C04B 2235/5445: submicron sized, i.e. from 0,1 to 1 micron
- C04B 2235/656: characterised by specific heating conditions during heat treatment
- C04B 2235/658: Atmosphere during thermal treatment
- C04B 2235/6582: Hydrogen containing atmosphere
- C04B 2235/6584: at an oxygen percentage below that of air
- C04B 2235/6588: Water vapor containing atmospheres
- C04B 2235/768: Perovskite structure ABO3
- C04B 2235/77: Density
- C04B 2235/786: Micrometer sized grains, i.e. from 1 to 100 micron
- C04B 2235/96: Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- Y10T 29/42: Piezoelectric device making
- H10N: ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- C04B: LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE {(roofing granules E04D7/005)}; CERAMICS (devitrified glass-ceramics C03C10/00); REFRACTORIES; TREATMENT OF NATURAL STONE
- Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION

## Abstract

A method for producing a piezoelectric component is disclosed. In an embodiment, the method includes producing a ceramic precursor material of the general formula Pb1-x-y-(2a-b)/2V(2a-b)/2″BaxSry[(TizZr1-z)1-a-bWaREb]O3, where RE is a rare earth metal and V″ is a Pb vacancy, mixing the ceramic precursor material with a sintering aid, forming a stack which includes alternating layers including the ceramic precursor material and a layer including Cu and debindering and sintering the stack thereby forming the piezoelectric component having Cu electrodes and at least one piezoelectric ceramic layer including Pb1-x-y-[(2a-b)/2]-p/2V[(2a-b)/2-p/2]″CupBaxSry[(TizZr1-z)1-a-bWaREb]O3, where 0≤x≤0.035, 0≤y≤0.025, 0.42≤z≤0.5, 0.0045≤a≤0.009, 0.009≤b≤0.011, and 2a>b, p≤2a−b.

## Claims

### Claim 1

A method for producing a piezoelectric component, the method comprising:
producing a ceramic precursor material of the general formula Pb1-x-y-(2a-b)/2V(2a-b)/2″BaxSry[(TizZr1-z)1-a-bWaREb]O3, where RE is a rare earth metal and V″ is a Pb vacancy;
mixing the ceramic precursor material with a sintering aid;
forming a stack which includes alternating layers comprising the ceramic precursor material and a layer comprising Cu; and
debindering and sintering the stack thereby forming the piezoelectric component having Cu electrodes and at least one piezoelectric ceramic layer comprising Pb1-x-y-[(2a-b)/2]-p/2V[(2a-b)/2-p/2]″CupBaxSry[(TizZr1-z)1-a-bWaREb]O3, where 0≤x≤0.035, 0≤y≤0.025, 0.42≤z≤0.5, 0.0045≤a≤0.009, 0.009≤b≤0.011, and 2a>b, p≤2a-b.

### Claim 2 (depends on 1)

The method according to claim 1, wherein producing the ceramic precursor material comprises:
providing a mixture of starting materials, the mixture of starting materials are selected from the group consisting of Pb3O4, TiO2, ZrO2, WO3, RE2O3, BaCO3 and SrCO3;
calcining the mixture at a first temperature and milling the mixture to a first average diameter; and
calcining the mixture at a second temperature that is higher than the first temperature.

### Claim 3 (depends on 2)

The method according to claim 2, wherein the mixture obtained by mixing the ceramic precursor material with the sintering aid is milled to a second average diameter that is smaller than the first average diameter.

### Claim 4 (depends on 3)

The method according to claim 3, wherein the mixture obtained by mixing the ceramic precursor material with the sintering aid further comprises adding Cu2O with a fraction of 0.05 to 0.1 mol %.

### Claim 5 (depends on 1)

The method according to claim 1, wherein mixing the ceramic precursor material comprises adding PbO or Pb3O4 as the sintering aid, a fraction selected for the sintering aid being between 0.5 and 3 mol %, based on 1 mol of ceramic precursor material.

### Claim 6 (depends on 1)

The method according to claim 1, wherein forming the stack comprises applying Cu to the layer comprising the ceramic precursor material by sputter-coating with Cu or printing with a Cu paste.

### Claim 7 (depends on 1)

The method according to claim 1, wherein debindering the stack takes place under steam with exclusion of oxygen.

### Claim 8 (depends on 1)

The method according to claim 1, wherein sintering the stack takes place at an oxygen partial pressure which lies between an equilibrium partial pressure of PbO/Pb and an equilibrium partial pressure of Cu/Cu2O.

### Claim 9 (depends on 8)

The method according to claim 8, wherein the oxygen partial pressure is set by a mixture of steam and forming gas.

### Claim 10 (depends on 1)

The method according to claim 1, wherein sintering takes place at a temperature between 1000° C. and 1050° C.

### Claim 11 (depends on 1)

The method according to claim 1, wherein x=0.0295, y=0.0211, z=0.475, a=0.00753, b=0.0095, and RE=Yb are selected, and wherein debindering and sintering the stack comprises producing a piezoelectric ceramic layer comprising Pb0.945V0.00128″Cu0.003Ba0.0295Sr0.0211[Ti0.467Zr0.516W0.00753Yb0.0095]O3.

### Claim 12

A method for producing a piezoelectric component, the method comprising:
providing a mixture of starting materials, the mixture of starting materials are selected from the group consisting of Pb3O4, TiO2, ZrO2, WO3, RE2O3, BaCO3 and SrCO3;
calcining the mixture at a first temperature and milling the calcinated mixture to a first average diameter;
calcining the calcinated mixture at a second temperature that is higher than the first temperature and forming a green body;
forming a metal layer on the green body;
forming a stack of green bodies and metal layers;
debindering the stack; and
sintering the stack thereby forming the piezoelectric component with piezoelectric ceramic layers comprising Pb1-x-y-[(2a-b)/2]-p/2V[(2a-b)/2-p/2]″CupBaxSry[(TizZr1-z)1-a-bWaREb]O3, where RE is a rare earth metal and V″ is a Pb vacancy, where 0≤x≤0.035, 0≤y≤0.025, 0.42≤z≤0.5, 0.0045≤a≤0.009, 0.009≤b≤0.011, 2a>b and p≤2a-b.

### Claim 13 (depends on 12)

The method according to claim 12, wherein forming the metal layer comprises sputtering the metal layer.

### Claim 14 (depends on 12)

The method according to claim 12, wherein the metal layer comprises a Cu layer.

### Claim 15 (depends on 12)

The method according to claim 12, further comprising mixing the mixture calcinated at the first temperature with a sintering aid.

### Claim 16 (depends on 15)

The method according to claim 15, wherein mixing the mixture calcinated at the first temperature with the sintering aid comprises adding PbO or Pb3O4.

### Claim 17 (depends on 15)

The method according to claim 15, further comprising milling a mixture obtained by mixing the mixture calcinated at the first temperature with the sintering aid to a second average diameter that is smaller than the first average diameter.

### Claim 18 (depends on 12)

The method according to claim 12, wherein debindering the stack comprises steaming the stack with exclusion of oxygen.

### Claim 19 (depends on 12)

The method according to claim 12, wherein sintering comprises heating the stack to a temperature between 1000° C. and 1050° C.

### Claim 20 (depends on 12)

The method according to claim 12, wherein debindering and sintering the stack comprises producing the piezoelectric component comprising Pb0.9451V0.00128″Cu0.003Ba0.0295Sr0.0211[Ti0.467Zr0.516W0.00753Yb0.0095]O3.