NASA/CR-2001-211225 ICASE Report No.

2001-28

_i!ili i

Piezoelectric
T.L. Jordan NASA Langley

Ceramics

Characterization

Research

Center,

Hampton,

Virginia

Z. Ounaies ICASE, Hampton, Virginia

September

2001

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NASA/CR-2001-211225 ICASE Report No. 2001-28

Piezoelectric
T.L. Jordan NASA Langley

Ceramics

Characterization

Research

Center,

Hampton,

Virginia

Z. Ounaies ICASE, Hampton, Virginia

ICASE NASA Langley Research Center Hampton, Operated Virginia by Universities Space Research Association

National

Aeronautics

and

Space Administration Langley Research Center Hampton, Virginia 23681-2199 Prepared for Langley Research Center under Contract NAS 1-97046

September

2001

Available

from the following: Information (CASI) National Technical Information Service (NTIS)

NASA Center for AeroSpace 7121 Standard Drive Hanover, MD 21076-1320 (301) 621-0390

5285 Port Royal Road Springfield, VA 22161-2171 (703) 487-4650

PIEZOELECTRIC

CERAMICS
T. L. JORDAN

CHARACTERIZATION
2

1 AND Z. OUNAIES

Abstract. polycrystalline

This review ceramics;

explores

piezoelectric single crystals,

ceramics polymeric

analysis materials

and

characterization.

The

focus is on are

therefore,

and organic/inorganic polycrystalline

composites

outside the scope of this review. To thoroughly understanding the history relations

grasp the behavior

of a piezoelectric

ceramic, a basic of

of the ceramic itself should not be overlooked. of piezoelectricity and a discussion on processing

To this end, we have presented of the ceramic

a brief introduction

and development

of the constitutive

that

define methods

the behavior

of a piezoelectric parameters

material. of interest.

We have attempted Excellent

to cover the most common coverage of

measurement

as well as introduce

sources for more in-depth

specific topics can be found in the bibliography. some of the concepts Subject

In most cases, we refer to lead zirconate

titanate (PZT) to illustrate

since it is the most widely used and studied piezoelectric Structures and Materials ceramic, ferroelectricity,

ceramic to date.

classification.

Key words, piezoelectric

piezoelectricity,

crystalline

piezoelectric

coefficient,

hysteresis,

poling,

characterization Materials: History and Processing. Smart materials are materials that undergo

1. Piezoelectric

transformations through physical interactions. An alternate definition a change in its environment Piezoelectric electrorheological materials, and through the use of a feedback shape-memory alloys, of currently

is that a smart material is a material that senses such a change. materials,

system, adapts to correct or eliminate materials, magnetostrictive

electrostrictive

fluids are some examples

available smart materials. for pressure. It follows that a piezoelectric stress (or pressure), material develops

Piezoelectricity a potential

stems from the Greek wordpiezo when subjected

across its boundaries

to a mechanical deformation

and vice versa, when an therefore fall in the polarization exists

electric field is applied to the material, class of smart materials. that can be reoriented 1.1. Definition solid. Some ceramic Ferroelectricity

a mechanical

ensues. Piezoelectric

materials

is a subgroup

of piezoelectricity,

where a spontaneous

by application of an AC electric field. and History. materials Piezoelectricity become is a linear effect that is related to the microscopic polarized when they are strained; structure of the

electrically

this linear and reversible by

phenomenon

is referred to as the direct piezoelectric

effect. The direct piezoelectric strained

effect is always accompanied

the converse piezoelectric origin of the piezoelectric external However symmetric.

effect where a solid becomes effect is the displacement

when placed in an electric

field. The microscopic In the absence of is zero.

of ionic charges within

a crystal structure.

strain, the charge distribution when an external A net polarization

within the crystal is symmetric the charges are displaced

and the net electric and the charge

dipole moment distribution

stress is applied,

is no longer

develops and results in an internal

electric field. A material

can only be piezoelectric

if the unit cell has no center of inversion. Piezoelectricity is a property possessed by a group of materials, discovered in 1880 by Pierre and Jacques

Curie during their study of the effects of pressure tourmaline, and Rochelle salt. In 1881, the term

on the generation "piezoelectricity"

of electrical

charge by crystals such as Quartz, by W. Hankel, and the

was first suggested

1 M/S 238, NASA Langley Research Center, Hampton, VA 23681. 2 ICASE, M/S 132C, NASA Langley Research Center, Hampton, VA 23681-2199. This research was supported by the National Aeronautics and Space Administration under NASA Contract No. NAS1-97046 while the second author was in residence at ICASE, NASA Langley Research Center, Hampton, VA 23681-2199.

converse

effect was deduced by Lipmann scientific community

from thermodynamics established

principles.

In the next three decades, collaborations and by 1910, Voigt's the complex "Lerbuch

within the European der Kristallphysic" relationships

the field of piezoelectricity; reference work detailing

was published

and became a standard

electromechanical made it difficult ultrasonic

in piezoelectric

crystals [ 1]. However, the complexity until a few years later. Langevin

of the science of piezoelectricity et al. [2] developed for piezoelectric transducers, dihydrogen

for it to mature to an application transducer applications etc...In during

a piezoelectric materials

World War I. Their success

opened up opportunities such as ultrasonic

in underwater accelerometers,

as well as a host of other applications discovered

microphones, phosphate

1935, Busch and Scherrer

piezoelectricity

in potassium

(KDP). The KDP

family was the first major family ofpiezoelectrics During World War II, research until then, breakthrough respectively. limited performance in piezoelectric

and ferroelectrics materials inhibited

to be discovered. to the U.S., the Soviet Union and Japan. Up but that changed when a major

expanded

by these materials

commercialization

came with the discovery of barium titanate These families of materials of tailoring exhibited

and lead zirconate

titanate

(PZT) in the 1940s and 1950s properties. Furthermore,

very high dielectric

and piezoelectric and applications

they offered the possibility

their behavior

to specific responses materials.

by the use of dopants. available structure

To date, PZT is one of the most widely used piezoelectric ceramics

It is noted that most commercially structure (Figure 1). The perovskite are linked together

(such as barium titanate and PZT) are based on the perovskite arrangement where the corner-sharing

(ABO3) is the simplest

oxygen octahedra

in a regular

cubic array with smaller cations (Ti, Zr, Sn, Nb etc.) occupying the central Ba, Sr, Ca, Na etc.) filling the interstices PbTiO3, PbZrO3, NaNbO3 between octahedra

octahedral

B-site, and larger cations (Pb, such as BaTiO3, ferroelectric substitutions and on the

in the larger

A-site. Compounds

and KNbO3 have been studied at length exploited. of useful etc. This structure though more

and their high temperature also allows for multiple complex compounds

antiferroelectric A-site and

phases have been extensively resulting in a number

B-site

such

as (Ba,Sr)TiO3,

(Pb, Sr)(Zr,Ti)O3,

Pb(Fe, Ta)O3, (KBi)TiO3

Ti, Zr

Fig 1o

Perow'kite

structure

Starting opening nations,

around

1965, several Japanese markets

companies

focused on developing devices. The success applications

new processes

and applications, effort attracted

and other

new commercial

for piezoelectric

of the Japanese

and today the needs and uses extend and the automotive field.

from medical

to the communications

field to military

applications

A review oftheearly history ofpiezoelectricity is found theworkofW.G. ady in C [3];andin 1971 Jafl_, Cook andJaffe published thebook "Piezoelectric Ceramics" [4]thatisstillone ofthemosteferenced on r works piezoelectricity. 1.2. iezoelectric P
powder preparation. processed to mechanically and properties and poling: Ceramic Processing. The fabrication of most bulk piezoelectric ceramics starts with The powder is then pressed to the required strong and dense ceramics. are powder preparation, shapes and sizes, and the green shapes are in turn processes that influence the product

The more important

characteristics electroding

powder calcining

and sintering.

The next steps are machining,

application

of a DC field to orient the dipoles and induce piezoelectricity. is the mixed oxide route. In this process, powder is prepared titanate from the lead are

The most common appropriate stoichiometric

powder preparation mixture

of the constituents'oxides.

In the case of lead zirconate Depending on application,

(PZT):

oxide, titanium

oxide, and zirconium

oxide are the main compounds. PZT ceramics

various dopants

used to tailor the properties some of their properties. lower the piezoelectric applications.

of interest.

are rarely utilized

without the addition

of dopants to modify but also

A-site additives coefficients;

tend to lower the dissipation

factor, which affects heat generation,

for this reason

they are mostly used in ultrasonics coefficients

and other high frequency constant etc. and loss.

B-site dopants as actuators

increase the piezoelectric in vibration

but also increase the dielectric optical positioning PZT ceramics.

They are utilized

and noise control, benders, oxide route for making

application

Figure 2 shows a flowchart done by dry-ball milling faster than dry-milling; for making

of the mixed

Mixing

of the powders can be wet ball-milling is

or wet ball milling, both methods having however, the disadvantage wet-ball

advantages

and disadvantages:

is the added step of liquid removal. ethanol and stabilized zirconia

The most common media

method

PZT ceramics

is through

milling;

are added for a wet

milling process.

A vibratory mill may be used rather than a conventional

ball mill; it was shown by Herner [5] that media are used to further reduce the of PZT ceramics; it is important that any

this process reduces the risk of contamination contamination risks. The calcination be complete

by the balls and the jar. Zirconia

step is a very crucial step in the processing phase forms during

the crystallization

and that the perovskite left after mixing;

this step. The goals are to remove

organics, water or other volatiles the ceramic is processed and after sintering. After calcining, for binder burn-out

to react the oxides to form the desired phase composition and allow for better homogeneity

before during

to useful devices; and to reduce volume shrinkage

a binder is added to the powder, and densification. in the sintering

then the mixture

is shaped usually by dry-pressing

in a die for

simple shapes, or extrusion,

or casting for more complicated

bodies. Next, the shapes are sintered:

placed in an oven

The major problem this problem, crucibles.

of the PZT ceramic in the presence

is the volatility of a lead source,

of PbO at about 800C.

To minimize

the PZT samples

are sintered

such as PbZrO3, and placed in closed

The saturation

of the sintering

atmosphere varying

with PbO minimizes between 1200-1300C.

lead loss from the PZT bodies. Sintering Despite precautions, there is usually a

can now be carried resulting

out at temperatures

loss of 2%-3%

of the initial lead content. into desired shapes, electrodes ceramic. are applied and a strong DC field is used to orient or at higher temperatures aligns the dipoles in a

After cutting and machining the domains depending in the polycrystalline on the material and

DC poling can be done at room temperature The poling process only partially

the composition. polarization

polycrystalline

ceramic, and the resulting

is lower than that for single crystals.

PbO, I MIXING dopants

TiO2,

ZrO2 1

of needed if OXIDES:

I Zirconia media + Ethanol WET MILLING 24 hrs

SIEVING for BETTER MIXING and DRYING REDUCTION 12 HRS SIZE AT 80C,

READY

for CALCINING

F_g 2.

Mixed-oxide

route

of preparing

PZT

This processing techniques properties

technique

presents

many uncertainties

and the presence

of a wide number of other fabrication PZT ceramics with optimum This problem is process, which

is an indication and microstructure.

that there is a great need for the production One problem often encountered

of reliable

is the deviation

from stoichiometry. the sintering

often due to impurities invariably

present

in the raw materials alterations

as well as the lead loss during

results in substantial

of the PZT properties.

As a result, the elastic properties 20% within

can vary as much [6]. Also, the It is the if not

as 5%, the piezoelectric piezoelectric important constituents impossible. and Moulson precipitation in powder piezoelectric and dielectric then that

properties properties

10% and the dielectric generally

properties

the same batch

suffer if there is any lack of homogeneity mixed. In the method mixing

due to poor mixing. above, however, is difficult

the constituent

oxides be intimately

described

are solid solutions More information

and it has been shown that an intimate on the preparation of piezoelectric

of solid solutions

ceramics can be found in Jaffe, Cook and Jaffe [4], methods including hydrothermal processing and co-

and Herbert [7] among methods are described

others. Other processing in references

[8-10]. It is noted that there has been a great deal of development that has resulted in further expanding the application of

processing, ceramics.

shaping

and sintering

[11,12,13]

1.3. Ferroelectricity. spontaneous temperature polarization

Some piezoelectric that can be reversed materials

materials

are also ferroelectric. by application

A ferroelectric

material

possesses

in direction

of a realizable

electric

field over some

range. Most ferroelectric

have a Curie Temperature,

To below which they are polar and above decreases according to the Curiematerials are

which they are not. The dielectric

permittivity

often has a peak at To and linearly

Weiss law above it [4,7]. The very large permittivity greatly exploited Applying ferroelectric in many applications, a large alternating loop, relating

values that are characteristics

of ferroelectric

most widely in the multilayer-capacitor electric field causes the polarization

industry. to reverse, and this gives rise to the

hysteresis

the polarization

P to the applied

electric field E. A typical field-polarization

loop isillustrated Figure.Atlarge in 3 signals, theelectric both displacement D and

functions of the field E. They are related to each other through D i = P_ +eoE where eo is the permittivity equation (1) is negligible, of free space ( 8.85xl _ the linear equation

the polarization below (1)

P are non-linear

0 -12

C/V-m).

For most ferroelectric

ceramics,

the second term in of the P-E materials.

and a D-E loop and P-E loop become interchangeable. polarization

Two key characteristics

loop are the coercive field Ec and the remanent Ec is the field at which the polarization

Pr, both defined by analogy to ferromagnetic

is zero. Pr is the value of the polarization will have a polarization

when the electric field is zero. both

Once the field is switched off, the material P_ and Ec can be determined.

equal to P_. Once the P-E loop is saturated

A loop is said to be saturated

once the values of P_ and Ec no longer vary.

Pr_.__ _
eo .m N .m m O _Oev

o__

\
E
c

__8_
I I I I

Electric

Field

F_g

3.

Hysteresis

loop

of a poled

piezoelectric

ceramic

Generally, ferroelectric.

the existence

of the P-E loop is considered circuit [14] or a modified sample;

as evidence

towards

establishing

that a material

is

A Sawyer-Tower

version of it, is commonly

used to obtain a P-E loop. An bymeans of

AC voltage is applied to the electroded a large reference the capacitor; capacitor

the resulting

charge stored on the sample is determined

placed in series with the sample. An electrometer this voltage with the value of the reference

can be used to detect the voltage across capacitor, the charge across the sample

by multiplying

results. that

The

reference

capacitor loops

should

be 100 to 1000 frequency

times

the value

of the capacitance dependent.

of the sample.

It is noted

ferroelectric In addition

hysteresis

are both

and temperature leads

to the P-E loop, polarization is shown in Figure field 4. The

switching shape

to strain-electric that of a butterfly, effect walls

field hysteresis. and dictates start

A typical referred

strain-field to as the As the on

response "butterfly field

curve loop".

resembles

it is often

As the electric the strain

is applied, linear

the converse with the field

piezoelectric as domain

that a strain

results.

is increased,

is no longer should consult

switching.

For more

sources

ferroelectricity,

the reader

the bibliography

[15-19].

T
e.m L,. o

09
%

8 _ o g_
o

g_
o

Nd

Electric

Field

---_

Fig

4.

Butterfly

loop

indicating

switching

2. Constitutive structure in average atoms of the material. diameter)

Relations To better from

and

Materials

Property.

An

understanding crystallite is made

of piezoelectricity (small single crystal

begins less than

with

the

explain

it, let us consider ceramic. unit This

a single crystal

100gm charged the

a polycrystalline positions

up of negatively symmetry 32 classes

and positively

occupying

specific

in a repeating

or cell.

The specific into

of the unit or point

cell determines groups (from

possibility crystal classes, symmetry, symmetry

of piezoelectricity systems: triclinic, possess

in the crystal. monoclinic, a center

All crystals

can be divided tetragonal,

7 basic 32 of of

orthorhombic, of symmetry, of the

rhombohedral, (one symmetry respect

hexagonal class,

and

cubic). lacking

Of the a center of center

21 do not is not means

and 20 are piezoelectric combination of other

although The other

piezoelectric

because

elements). to each

lack

that a net movement

of the positive

and negative

ions with

as a result

of stress

produces electric ipole. heceramic, an d T beingcomposed therandom of orientation these of piezoelectric crystallites, inactive, is i.e.,the effects fromthe individual crystalsancel ach c e otherandno discernable piezoelectricity is present. Regions ofequally riented o polarization vectors areknown asdomains. "Poling" a is commonly method used toorienthedomains t bypolarizing theceramic through application the ofastatic electric field.The electrodes applied are totheceramic asufficiently and highelectric fieldisapplieduch thedomains s that rotate nd a switch inthedirection oftheelectric The field. result isnever fullorientation a ofalldomains; however the polycrystalline exhibits ceramic alarge piezoelectric During process, isasmall effect. this there expansion ofthe material thepoling along axisand acontractionboth in directions perpendicular (see toit Figure 5).Withalarge number ofallowable directions asnearhemorphotropic boundary polar such t phase (where theZrto Ti ratiois equal to48to 52), hemaximum t deviation ofthepolar axisofa grain from theaverage direction ill be polar w smaller, theloweringfthepolarization and o willbeminimized assuming optimumlignment. a

V=O

V=n

I_',"__'_./x, ''_

I
Fig 5. Poling of a piezoelectric, ferroelectric

T
ceramic

I,,',-' I

"

-"

t6
15_ 2 Fig 6. Reference axes

2.1. Constitutive be taken of changes

Relations.

When writing the constitutive displacement

equation

for a piezoelectric directions

material,

account must

of strain and electrical

in three orthogonal

caused by cross-coupling axes are

effects due to applied electrical shown in Figure 6.

and mechanical

stresses. Tensor notation is first adopted, and the reference

The state of strain is described rank tensor Te. The relationships then fourth rank tensors.

by a second rank tensor X;, and the state of stress is also described the stress tensor to the strain tensor, compliance between the electric field Ej(first rank

by a second

relating

si;e, and stiffness ci;e, are tensor) and the electric

The relationship

displacement D_(also a first rank tensor) is the permittivity equations are therefore written as: T D_ =e_Ej

_7, which

is a second rank tensor.

The piezoelectric

(2)
+ d_kT;k

SUklTkl where d/j k ,d/j k are the piezoelectric constants (third rank tensor). Superscripts

(3)
T and E denote that the dielectric

constant ei; and the elastic constant s_jklare measured under conditions of constant stress and constant electric field respectively. In general, a first rank tensor has three components, a second rank tensor has nine components, a third rank tensor independent. properties number Figure has 27 components and a fourth rank tensor has 81 components. are orientation-dependent; of the material. A convenient they describe Not all the tensor a set of equations components that are

Both these relations

relate these

in different orientations of independent components.

The crystal symmetry way of describing direction

and the choice of reference

axes reduce the as given by by the

them is by using axis directions the shear planes

6. The convention

is to define the poling

as the 3-axis,

are indicated

subscripts introduced (i (i

4, 5 and 6 and are perpendicular above, where a 3-subscript tensor

to directions notation

1, 2 and 3 respectively. 1,2,3) is replaced (i,j

This simplifies by a 2-subscript

the notations notation

(i,j,k

matrix

1,2,3 and j 1,2,3,4,5,6), 1,2,3,4,5,6).

and a 2-subscript

tensor notation

1,2,3) is replaced by a 1-subscript

matrix notation orthogonal (field or

A shear strain such as $4 is a measure

of the change

of angle between the two initially gives the "electrical" deformation

axes in the plane perpendicular dielectric isotropy parallel displacement) of poled ceramics to the poling

to axis 1. The first subscript

of the d-constant

direction

and the second is expressed

gives the component in their piezoelectric

of mechanical constants

or stress.

The planar

by the equalities

d32 d31 (an electric field

axis 3 interacts

in the same way with axial stress along either the 2-axis or the 1-axis) and in the same way with a shear in the 2,3-plane as a field along

d:4 d15 (an electric field parallel

to the 2-axis interacts

the 1-axis with a shear in the 1,3-plane). plane perpendicular 2.2. Property piezoelectric matrix to the polar axis. Matrix for a Poled

Similar relations hold for the elastic constants

because of the isotropy in the

Piezoelectric

Ceramic.

A piezoelectric crystals.

ceramic

has only one type of isotropic. This is

regardless

of the symmetry

of the constituent

The ceramic is initially to the poling direction,

isotropy is destroyed in the poling direction. transversely an infinite described isotropic. The symmetry elements

In the directions

perpendicular

the material

are an axis of rotation

of infinite order in the direction notation,

of poling and is

set of planes parallel as _mm

to the polar axis as reflection to the hexagonal matrices

planes. In crystallographic

this symmetry

and is equivalent dielectric

polar crystal class, 6mm. for the cylindrical symmetry of poled PZT are shown in the constants such asg_;

The elastic, equations (described

and piezoelectric analogous

below. Matrices

to the piezoelectric

one also apply to other piezoelectric

in the next section).

$11

$12

$13

0 0 0

0 0 0

0 0 0 0 0 2(sll -s12)
(4)

$12 $13

$11 $13

$13 $33

0 0 0

0 0 0

0 0 0

s44 0 0 0
$44

e1 0 0 0 el 0

0 0 e3 (5)

0 0

0 0

0 0

d15 0 0 (6)

d15 0

g31 g31 d33 0

For the symmetry equations below:

of poled ceramics

then,

the general

equations

(1) and (2) are replaced

by the specific

D 1 = e 1 E 1 + d 15 T 5

(7)

02=

E.2E

2 +dsT

(g)

D3=

e E
E

+d
E

(T+TJ+d
E L-_-_I3 T+d

(9)

S1

--

_ii

TI-_-_I2

(10)

E 2

Sll

T+s 2
E

12

T 1 +s

13

T 3 +d

31

E3(ll)

S = s
E

(T+TJ+s
T 4 +d
E

T+dE
E2

(12)

S 4 =s

44

15

(13)

S 5 =s

44 E

T 5 +d
T6

15

E1

(14)

S 6 = s 66 Equations

(15)

(7)-(9) relate to the direct effect, equations

(10)-(15)

relate to the converse

effect.

3.Piezoelectric Parameters: Definitions

considering the electromechanical

and Characterization.

The parameters

that are of interest charge coefficients

when

effects of piezoelectric

materials are the piezoelectric

(d31 and

dss), the piezoelectric voltage coefficients (gsl and gss) and the piezoelectric coupling factors (ks1, kss , k and _). The d-coefficient is the proportionality constant between electric displacement and stress, or strain and electric field (equations vibrational (2) and (3)). High d-coefficients applications. The g-coefficient are desirable in materials utilized as actuators, such as in motional and

is related to the d-coefficient

by the following expression:

dm i

T = enmgni

(16) are desirable in materials intended to be used as sensors, to

where m,n

1, 2, 3 and i

1, 2, ...6. High g-coefficients to mechanical coupling stress.

produce voltage in response The piezoelectric

factor k is a measurement

of the overall strength

of the electromechanical

effect.

It is often defined as the square root of the ratio of electrical the case of the direct effect) converse or the mechanical energy

energy output to the total mechanical to the total electrical

energy input (in

available

energy (in the case of the is always incomplete. constant e (F/m) and

effect). The value of k is of course always less than unity because energy conversion Other important properties of PZT are the dielectric tan6. The dielectric The dielectric properties, namely the dielectric
-12

the dissipation material constant brought

factor or loss tangent to a given voltage.

constant

is a measure

of the charge stored on an electroded F/m. The relative dielectric In case of

constant constant")

of vacuum is eo 8.85x10

K (often referred to as just "the dielectric constant

is the ratio ofe and eo, and is dimensionless. part; the loss tangent is defined

ac field, the dielectric the imaginary

has both a real part and an imaginary

as the ratio of

part to the real part. of these constants constant depend on the PZT compositions. near the morphotropic As an example, phase boundary the d-constants, g-

The values constants

and the dielectric

for compositions

show their highest for most

values on the tetragonal compositions;

side of the transition

[4]. It is then possible to tune the values of these properties adding dopants to the PZT formulation.

one way of achieving Method

that is through Circuit

3.1. Resonant

and Equivalent

3.1.1. Resonance resonate.

method.

Any body of mass has certain

characteristic

frequencies

at which

it prefers

to

When excited at this resonant Following

frequency, J_, the body will resonate frequency amplitude frequencies is an anti-resonant is at a minimum. provides

freely with a greater amplitude

than at of the

other frequencies.

this resonant

frequency, J_, where the impedance Piezoelectric to evaluate ceramics

body is at a maximum the measurement properties

and the oscillation

are no different and and elastic

of these characteristic Different

the means

the piezoelectric or planar,

of the ceramic. constants ceramic impedance

modes of vibration

of the ceramic, resonance 7.

such as thickness plot of impedance

give insight to for a

the different piezoelectric minimum

associated near

with that mode. is shown

A typical in Figure

versus frequency

a resonance

Notice the resonant

frequency, J_, at the point of

and the anti-resonant

frequency, J_, at the point of maximum

impedance.

10

T
N

_E

Frequency, f

F_g

7.

Impedance

of a piezoelectric

ceramic

at resonance

Fig8.

Resonant

equivalent

circuit

of a piezoelectric

vibrator

At resonance, commonly alternate

a piezoelectric

element may be modeled by the equivalent

circuit as shown in Figure 8. This circuit is on Piezoelectricity [20]. An

referred to as Van Dyke's Model and is recommended model, proposed as complex All discussion by Sherrit et al. [21], eliminates to better characterize presented

by the IEEE Standard

the resistance,

R1, and instead represents piezoelectric

the remaining especially

components polymers.

the losses associated Van Dyke's

with certain Model.

elements,

below will assume

BelowJ_

and aboveJ_,

the ceramic

behaves capacitively;

however between these two frequencies, Additionally, modes. the resonance

the ceramic behaves inductively. isolated

This model is only

valid near the resonance. the effects of any adjacent Geometries Fixturing suitable of the

must be sufficiently of the resonance,

from other modes to eliminate

To assure isolation the different not impose

sample geometry must be chosen carefully. are presented in Table 1. This can be

for measuring should

piezoelectric

and elastic coefficients on the vibration

sample

any constraints

of the ceramic.

11

accomplished byusing apoint older h positioned atanode fvibration. allleadshould o Also, s beshielded uptothe contact as point much possible as toavoid stray apacitances may any c which arise. Earlieriterature suggested circuits l has several tomeasureJ_ ofapiezoelectric andJ_ ceramic [22-25]. hese T circuits suallyonsist u c ofanoscillator forexciting thesample, avoltmeter orother evice d formeasuring current through thecircuit, nd a additional discrete components. TofindJ_, theoscillator varied frequency is in untilthe maximum current isdetected through thecircuit. imilarly, the S forJ_, frequency ofminimum current isdetermined. It shouldenoted b thatthere areactuallyix characteristic s frequencies thatmaybeidentified a particular for resonance includefnndre, which a thefrequencies ofmaximum minimum and impedance;J_ the andJ_, resonant and antiresonant frequencies; andre, parallel andJp the resonant frequency series and resonant frequency. Standard IEEE 177 [23]identifies sixfrequencies establishes these and thatformany ases, c includingiezoelectric p ceramics, one can make theassumption thatfn j_ J_ andJ_ f_. For lossymaterials, such as some of the piezoelectric thin
films, this assumption magnitude can introduce appreciable errors and the six frequencies by substituting should be considered an adjustable resistor separately. The of the minimum impedance, Zm, may be determined frequency into the circuit reading is the

for the ceramic at the previously same as for the ceramic. of measurement, the discrete

identified

and adjusting

the resistance

until the voltmeter available

Today, fully integrated

impedance

analyzers

are commercially

to make this type

and even allow the researcher of the equivalent

to choose an equivalent

circuit model and will report the values of Also, commercial to evaluate off- the shelf software is information and in the

components which

circuit along with J; andJ_. with an analyzer

now available calculate evaluation foundation

can be used in conjunction material properties

the impedance

the relative

of a piezoelectric a basic

device [26].

These tools can aid the researcher behavior

of material

properties,

however

understanding

of piezoelectric

is an important

that should not be overlooked.

Table Sample geometries'for measurement 1. of material properties

Dimensional

long,

slender,

length

thin,

flat plate,

thickness

poled;

thin

flat

disc,

thickness

poled

Requirements

poled

rod;

1 > 3d

l>3.5t,

d>lOt

K3

T ,

Properties Measured

k33 , tan 8, s3_,

K3 T , k31

, tan

a,

Sl_, T

K 3 ,kp,tan
s3E3, d33, g33, QM S E' d31, g31, QM

_,QM

12

3.1.2. Measurement of material

low excitation voltage voltages (mV level). [27,28], the and frequency

properties. Although lkHz,

Capacitance research

measurements

are usually carried out at lkHz and at and loss to vary with excitation in the determination of material to the

has shown capacitance measurement is used

low voltage

properties. permittivity

The free relative of free space.

dielectric

constant,

K r, is defined as the ratio of the permittivity

of the material

It is calculated

from the following: K r _ tC eo A (17)

where t is the distance between space (8.85

x 10 -12 F/m),

electrodes

in meters,

C is the capacitance in meters 2.

in farads,

6 o is the permittivity

of free

andA

is the area of an electrode

The loss tangent,

tan6, is defined of the dielectric when operated

as the ratio of resistance losses in the material under dynamic

to reactance and therefore

in the parallel also a measure

equivalent

circuit of

Figure 9a. It is a measure capacity of the ceramic

of the heat generation and is usually

conditions.

This is a direct measurement

formed at the same conditions

as the capacitance

measurement.

O-------

-------0

I
(-,p
(a)

,AA/Xr---R s C s

Fig 9. Non-resonant

(a) parallel

and (b) series

equivalent

circuit

The three most common subscripts are for length

coupling

coefficients

are kp, ks1, and kss; where thep extensional modes.

is for planar,

and the 31 and 33

extensional

and thickness

The coefficients

kss and ksl are calculated

from the frequencies

of minimum

and maximum

impedance

and are given by the equations

13

k33 2 1-_ (f"

2 -)

tan_-

2f.

._

(18)

L
k312 _ I]/

(19)

l+gt where: (20)

1ff=2(l+f"-f'_

)]tan(:C(f"-f')_ ) [

The planar

coupling

coefficient

kp is defined for thin discs and can be approximated kp =

by (21)

f) -f/ L'

Elastic compliance load (stress). whether constants

is the ratio of a material's

change in dimensions

(strain) in relation to an externally material, the compliance boundary

applied on

This is the inverse of Young's or perpendicular

modulus.

For a piezoelectric

depends

the strain is parallel are calculated

to the poling

axis and the electrical

conditions.

Elastic

from the following equations: D

$33 4

1 PI, t
D $33 -,_2.2

(22)

E $33

(23)
1 -k323

E
Sll-

1
2 2

(24)

4of,

S D

= sE0--k21)

(25)

where p is the density of the material ceramic. The superscripts

in kg/m 3 and 1 is the distance

between

electrodes

and w is the width of the electric field

D and E stand for constant

electric displacement

(open circuit) and constant

(short circuit) respectively. The at,?. piezoelectric coupling, constants, which relate the applied constant. electric field to the strain, can be calculated from the

elastic coefficients

and the dielectric

They are (26)

d33 = k3341?.oKfs3E3

d31

k31

;r_

(27)

The gij piezoelectric

constants

are related to the d_jcoefficients

by the following

equations:

14

i g33

d33

(28) eoK[

i g31

d31

(29) eoK[

It should be noted that the piezoelectric resonance and do not account for any non-linear

coefficients behavior

calculated

above are only valid at frequencies

well below

of the ceramic. however they will vary with the degree which must be determined of

They are not dependent polarization of the ceramic.

on the dimensions

of the material,

They also do not provide the sign of the coefficient,

through

direct measurements. The mechanical QM, the ratio of reactance to resistance in the series equivalent circuit of Figure 9a is given by:

Qv

--

2TOCrZmCol

--2_-2 {.j, jrfa2

(30)

3.2. Direct

Methods.

Direct

measurements

of the piezoelectric

constants

are possible

and have been used to the behavior and other input to the or a charge

quantify the direct and converse effects in ceramic samples. of the ceramic characteristics ceramic, in regards to hysteresis, non-linearity,

Direct methods response,

are also used to investigate aging, typically thermal behavior,

frequency

that are not resolved

by the above methods.

These methods

apply a known

either an electric

field or a force, and record the corresponding These methods above. are in contrast

output, either a deformation characterization

under various conditions. resonance techniques

to the bulk material

using the electrical

described

Many times, the direct measurements Typical processing

are carried out on a ceramic that has laminating, applying preload,

been configured mounting,

as a sensor or actuator.

may include electroding,

and other assembly procedures aid the researcher

to be able to effectively adapt the material in modeling the behavior of the piezoelectric

for use as a sensor or actuator. device and allow the efficient

These measurements integration

of the devices into real world applications. measurements of piezoelectric actuators are performed to determine the magnitude and sign of

Displacement the relationship this corresponds

between

applied electric

field and the strain developed, for bending type actuators

i.e., the converse effect. this relationship

For a PZT wafer, directly

to the 6/,)coefficient; properties

however

does not correlate

to any of the measured (10)-(15),

for out of plane bending

using the resonance

techniques.

Based on equations

it can be seen that for a case where the ceramic is free to expand (Tk field Ei and the 6/,). coefficient Sj = d,jE i

0), then the strain is only a function

of the product of the applied

(31)

Careful attention

must be paid to the boundary of applied

conditions

of the ceramic to assure that the above assumption

is

valid. In a plot of the strain as a function measurements actuator.

field, the slope yields an average transducer

value of d_j. Typically these on the

are made with a non-contacting

displacement

[29] to reduce the effects of loading techniques

Laser based and other optical or capacitive Displacements

displacement

measurement

are most commonly level for

used [30-32]. bending

may range from sub-micron

levels for single PZT wafers to the centimeter type measurement Direct

type actuators.

For very small displacements,

an optical-lever

system or interferometric application of either foil or

techniques

[33] have been used to resolve the displacement

of the ceramic.

15

optical strain gages also utilized has been formeasurement actuator These ofthe strain. measurements may bemade either tatically s ordynamically, depending measurement and onthe system theintended application oftheceramic. If dynamic measurements aremade, excitation frequencies beatleast norder fmagnitude thanany should a o less resonant frequency ofthedevice toassurelinear ehavior thattheboundary a b and conditions aresuitable forthe intended measurement. Another methodsed direct u tomeasure thepiezoelectric constantsbasednthedirect iezoelectric is o p effect [22,34].Here, known is either ppliedo or liftedoff a ceramictrest. The a load a t a resultingharge, c which accumulates ontheelectrodes, measured is then asavoltagecrosscapacitorparallel a a in withtheceramic orthe current theceramic beintegrated from can directly. is0(short IfEi circuit), equation then (2)reduces to:
D_ = dT zj and knowing the applied stress and measuring ceramic is immersed
j

(32) the appropriate dij coefficient can be found.

the electric displacement,

Ifa piezoelectric coefficient coefficient

in a liquid and the pressure of the liquid is varied, then the piezoelectric the voltage on a large capacitor pressure in parallel with the ceramic. This has

dh can be quantified represents the response

by measuring

of the ceramic to hydrostatic electrodes are perpendicular

applied equally in all axes. Convention The dh coefficient

dictated that for the dh coefficient, other d coefficients

to the 3-direction.

is related to the

for a ceramic by the equation: dh = d33 + 2d31 (33)

By varying frequency kilohertz (unimorph response

the frequency

of the excitation obtained.

voltage

to the ceramic

while

measuring

the displacement,

the

of the device maybe range depending

Typical resonant of vibration,

frequencies while

of bulk ceramic material frequencies actuator

are in the types

to megahertz or bimorph)

on the mode 100 hertz.

resonant

of bender

may be less than

For maximum

strain, a piezoelectric

can be excited at is to be used over a in both own

its natural frequency, range of frequencies. amplitude frequency and phase response

however this non-linear Also, careful attention distortion, when

behavior must be taken into account if the actuator must be paid to the instrumentation dynamic measurements. from the response materials. system's

dynamic response, systems

making

Measurement

have their

characteristics

which must be separated

of the ceramic under test. Hysteretic behavior is due to the lossy of the voltage

Hysteresis nature

is a phenomenon

that is present in all piezoelectric trails the applied

of the ceramic For actuators,

where the current

voltage by an angle c_ related is not only dependent To characterize

to the loss tangent on the excitation

material.

this means that the absolute

displacement

and frequency, in a ceramic, displacement The amount and minimum

but also on whether a sinusoidal vs. driving of hysteresis displacement voltage voltage, (usually

the voltage is increasing is applied as shown expressed

or decreasing.

the amount of hysteresis By plotting the

to the device

and the displacement behavior

is recorded.

in Figure in percent)

10, the hysteretic is defined

of the ceramic can be observed. between the maximum 10 is the fact that

as the largest difference

for any voltage divided by the total displacement. the amount of hysteresis also increases

Of note in Figure

as the peak voltage is increased,

for any given voltage.

16

250

200

150

100

0 -50 _-100 -150

1 1

-200

-250 -8 -6 -4 -2 0 DISPLACEMENT, mils 2 4 6 8

F_g 10.

Strain

hysteresis

of a piezoelectric

ceramic

unimorph

Generally,

piezoelectric

ceramic

actuators

exhibit

a decrease

in their

displacement

for a given excitation

voltage as they are loaded. increased, the displacement

This relationship eventually

can be seen in equation zero and the actuator amount

(3), for the case where Tk _ 0. As the load is provides only a force output. This force is To is To

reaches

known as the blocked force, and it is the maximum characterize measured. determine this relationship, the actuator

of force that the actuator can produce at that voltage.

is loaded with a load less than the blocked force and the displacement relationship can be determined (Figure 11).

If the load is varied, the blocked

then the force/displacement

force, the actuator

must be rigidly held so as not to deform, and the force output measured device. Because the displacement of some piezoelectric be calculated (34) actuators is quite below

with a load cell or other force-measuring small, this measurement can be difficult.

The blocked force FB can alternately FB E3d33wl E

$33

by the equations

FB -

E 3 d31 Wt

(35)

Sll

where E is the applied field, 1, w and t are the length, width and thickness applies to thickness Actuators pre-stressed extrapolating practical. completely extensional mode and equation

of the ceramic, respectively. extensional mode.

Equation

(34)

(35) applies to length thickness

with greater displacements or unimorph/bimorph

better lend themselves type actuators).

to the blocked force measurement The blocked force may also

(such as domed be determined by is not

actuators

the force/displacement In most constrained applications, state.

relationship actuators

to zero displacement somewhere

if a true blocked between

force measurement

will operate

the flee (unloaded)

state and the

17

T
Increasing
Fig 11. Typical stressstrain relationship for a piezoelectric ceramic

It has been previously the displacement reducing

reported

that a constant

preload

applied to a piezoelectric specimen [34-36].

actuator

can actually increase of simply This up to

of the ceramic

as compared

to an unloaded

This may be a result

the compliance

or mechanical

slop in a PZT assembly

or may be a real increase in the d-coefficient. as the pre-load is increased

effect will reach a maximum the blocked force. Temperature

and then start to cause a decrease in the coefficient

effects on the piezoelectric

coefficients

of ceramics

may also be evaluated.

Usually,

ceramics

must be used well below their Curie temperature Curie temperatures down to cryogenic

to maintain

polarization.

For hard and soft PZTs, the respective For operation at lower temperatures, temperature. even

are on the order of 360C (680 F) and 330C (626F). levels, the piezoelectric quantified through coefficients generally

decrease with decreasing

This effect

can be experimentally temperature range [34].

either resonance

techniques

or direct measurements

over the desired

The power required

to drive a piezoelectric P = 2nfC

tan

ceramic

can be calculated

from the following (36)

equation:

(_Vrms2

when the ceramic tangent,

is modeled

as in Figure

9a where f is the driving voltage.

frequency,

C the capacitance,

tan_ the loss

and Vm_ the root mean square of the excitation are assumed

Typically,

both the capacitance

and loss tangent of

the ceramic

to be constant when using equation of a ceramic.

(36). Doing so can lead to large errors when estimating supplied to the ceramic of capacitance and loss (36)

the power consumption should be measured of the material [28]. A number

To avoid these errors, either the voltage and current of the power consumption, or the variation

to provide a direct indication of applied

as functions

field and frequency

must be quantified

and incorporated

into equation

of researchers

have investigated

the power consumption between Research

characteristics motion

of PZT actuators of the structure

used to and the

excite a host structure electrical characteristics

[27,37,38]

and found a coupling actuator.

the mechanical by Brennan

of the piezoelectric materials

and McGowan

[27] shows that the of the coupling effects

power consumption of the host structure requirements

of piezoelectric

used for active vibration controlled.

control is independent

when the structure

is completely

From these findings, upon its geometry

they conclude

that the power and the

of the piezoelectric

actuator

are only dependent

and material

properties,

driving voltage and frequency are non-linear functions

of the control signal. Research and frequency

[23] has indicated of the excitation

that both capacitance voltage

and resistance

of the peak amplitude

18

Withtime, iezoelectric imparted p effects througholing degrade. ofpiezoelectric p will Aging ceramics, like many materials, other islogarithmic withtime.Withmost ceramics, a return toinitialperformance can levels be accomplished bysimplyepoling r thesample. levels Aging depend onthecomposition; thecouplingoefficient c of softPZT composition atarateof 1%pertimedecade ages versus2%forahardcomposition. Degradation of piezoelectric behavior depends also onthelevel fstress o towhich theceramic subjected. stress can is Large levels lead switchingfthepolarization to o andeventually depolingftheceramic. stresses induce o Large also micro cracking, can toceramic which lead breakage failure. and The methods outlined can above beused either separately ortogether toinvestigate thedielectric, piezoelectric, andelastic roperties ceramic. p ofa Resonant techniques, arethepreferred which methodfmeasurement o ofthe IEEEstandard, areeasyoimplement theassociated t and frequencies bemeasured can accurately. is even There commercially available hardware andsoftware available assist these easurements to in m andtheevaluation of material properties. However, methods these donotexplainny a non-linear behavior thatispresent intheceramic. Dependence ofmaterial properties onthefrequency amplitude appliedoltage among non-linear and ofthe v are these effects. irect easurements D m ofthepiezoelectric constants canquantify thematerial properties different under operating conditions provide and insight beyond thestandard behavior linear predicted resonance bythe techniques. These methods though, usually rigorous are more intheirrequirements ofmaterial handlingnd a instrumentation. 3.3. odeling f Piezoelectric M o Ceramics. There areahostofapplications forpiezoelectric materials and despite thefactthatthey have been studied forovera century, potential forimprovement andinnovation still persists. Modelingfpiezoelectric o ceramics theirproperties away and affords toaccelerate materials improvement and aidin deviceesignnd d a development. reason, Forthat wewould beremiss tomention albeit not it, briefly. This introduction isinnoway meant acomprehensive ofthevast ofmodeling as review area ofpiezoelectricity, however thereferences provide good cited a startinglace. must etaken p Care b todifferentiate between modelingfthe o piezoelectric material modeling "piezoelectric and ofa structure", often where apiezoelectric material islaminated oradhered toasubstrateaunimorph as orbimorph. A number ofresearchers experimented withcommercial packages asANSYS However, such [39]. these commercial packages limitations. groups written have Other have theirown codes withvaryingegrees d ofsuccess [40-43]. Finite element schemes combining piezoelectric acoustic and elements useful characterizing proved in the electromechanical ofpiezoelectric behavior transducers [44].Mostofthese schemes arerestricted thatthey in assume linearity fthecoefficients. etalexpanded o Perez onthese odels m byincludingonlinear n elements intothe equivalent [45].Modelsfthenon-linear circuit o hysteretic behavior ofpiezoelectric materials areabundantthe in literature, can and bedividedasednthedimensional they b o scale probe. Microscopic primarilytem models s from energy relations appliedttheatomic rmolecular [46].Macroscopic [47-49] ften a o level models o useempirical relations describe to thebehavior ofthebulkmaterial. Bothmethods theiradvantages have anddisadvantages; microscopic models require great umber a n ofparameters, notavailable, often andmacroscopic donot models consider theunderlying physics.number A ofauthors proposed athirdapproach, ameso-scale orsemi-microscopic model thatcombines theadvantages oftheprevious methods, allowing better thus a waytomodel thehysteretic behavior. isaccomplished This bystartingut rom o f energy principles appliedtthe a microscopic then level, using a relatively number small ofparameters tosimulate behavior the ofbulk ceramics [50,51]. 4.Conclusion. Characterization oftheelastic, dielectric andelectromechanical properties ofpiezoelectric ceramics iscrucial forseveral reasons. investigations First, ofthematerial properties provide linkbetween a the manufacturing process andceramic erformance. p Thisenables developer thematerials adjust the of to the manufacturing processf theceramic produce o to tailored materials. econd, S theengineer caninvestigate

19

prospective materialsor applicability a specific f to need. Also,material parameters obtained through characterization canbeused todevelop andvalidatenalytical a modelsftheceramics. o Insights gained through characterization ledtomany devices uses. orexample, have new and F investigation ofthehydrostatic coefficients ofPZT thosefthepiezoelectric and o polymer polyvinylidene fluoride, PVDF, identified product dh and gh as the of
a figure of merit and led to composite underwater and hydrophone research to combine both materials yielding a superior device that better fits ceramics have the applications. purposes. properties researchers More than a century Researchers continue after their discovery, to diligently uncover methods piezoelectric

become viable for commercial complex Recently, electromechanical as an example,

novel ways to characterize and applications single crystals

and as they do so, new processing at MIT have successfully Published

are revealed. [52], opening have become

grown piezoelectric processing

opportunities for newer applications. more abundant as well. Without engineering. 5. Acknowledgement. Research Center) question, piezoelectric

articles on composite

and characterization

ceramics

have secured a permanent

place in the field of material

science and

The authors express their sincere appreciation

to Dr. Jeffrey A. Hinkley (NASA Langley

for his review of the manuscript

and his helpful comments. REFERENCES

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REPORT

DOCUMENTATION

PAGE

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OMB No. 0704-0188

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Public reportingburdenfor this collection of informationis estimatedto average hour per response,ncludhTg time for reviewinginstructions, searchingexistingdata sources, ] i the gathering and maintainlngthe data needed,and completingand reviewingthe collectionof informatlon. Sendcommentsregardingthis burdenestimateor any other aspectof this collection of information, includingsuggestionsfor reducingthis burden, to Washington eadquarters H Services,Directoratefor InformationOperationsand Reports,1215 Jefferson DavisHighway,Suite 1204, Arlington, VA 222024302, and to the Office of Managementand Budget, PaperworkReductionProject (0704 0188), Washington, DC 20503. 1. AGENCY USE ONLY(Leave blank) 2. REPORT September 4. TITLE AND SUBTITLE ceramics characterization C NAS1-97046 WU 505-90-52-01 6. AUTHOR(S) T.L. Jordan and Z. Ounaies DATE 2001 3. REPORT Contractor TYPE AND DATES COVERED

Report 5. FUNDING NUMBERS

Piezoelectric

7. PERFORMING ICASE Mail NASA Hampton, Stop

ORGANIZATION

NAME(S)

AND ADDRESS(ES)

8. PERFORMING ORGANIZATION REPORT NUMBER ICASE Report No. 2001-28

132C Research 23681-2199 Center

Langley VA

9. SPONSORING/MONITORING National Langley Hampton, Aeronautics Research VA and Center 23681-2199

AGENCY Space

NAME(S)

AND

ADDRESS(ES)

Administration

10. SPONSORING/MONITORING AGENCY REPORT NUMBER NASA/CR-2001-211225 ICASE Report No.

2001-28

11. SUPPLEMENTARY Langley Technical Final Report To appear in tile

NOTES Monitor: Encyclopedia Dennis M. Bushnell Materials. 12b. DISTRIBUTION CODE

of Smart STATEMENT

12a. DISTRIBUTION/AVAILABILITY Unclassified Unlimited

Subject Category 34 Distribution: Nonstandard Availability: NASA-CASI (301) 621-0390

13. ABSTRACT (Maximum 200 words) This review explores piezoelectric therefore, single crystals, polymeric To thoroughly itself should not

ceramics materials

analysis and characterization. The and organic/inorganic composites

focus is on are outside

polycrystalline ceramics; the scope of this review. of the ceramic of piezoelectricity define tile behavior as well as introduce

grasp tile behavior of a piezoelectric be overlooked. To this end, we have on processing of the ceramic material. We have attempted sources zirconate ceramic

polycrystalline ceramic, a basic understanding presented a brief introduction of the history

and a discussion of a piezoelectric

and development of the constitutive relations that to cover the most common measurement methods in-depth (PZT) coverage to illustrate

parameters of interest. Excellent In most cases, we refer to lead used and studied piezoelectric

for more titanate to date.

of specific topics can be found in the bibliography. some of tile concepts since it is the most widely

14. SUBJECT poling,

TERMS crystalline ceramic, ferroelectricity, piezoelectric coefficient, hysteresis, piezoelectric characterization

15. NUMBER

OF PAGES

piezoelectricity,

27
16. PRICE CODE

A03
17. SECURITY CLASSIFICATION OF REPORT Unclassified NSN 7540-01-280-5500 18. SECURITY CLASSIFICATION OF THIS PAGE Unclassified 19. SECURITY CLASSIFICATION OF ABSTRACT 20. LIMITATION OF ABSTRACT

Standard Form 298(Rev. 2-89) Prescribed by ANSI Std. Z39 18 298 102