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NASA Te_caI Mem0mndum 102561 T Theory and ExperimentalTechnique for _NOndestrdctive Evaluation_Of ................ CeramicComposi_es _ -- i .... (NASA-TM-IO?56,1) THEORY AN_ EXP_-RTMt:NTAL N _0-23"/54 i_._:.-_>_5 '_'-_: TEC_4NTL_/IE FOR NqNDEST_UCTIVF- EVALUATIq_N GF __Z__ _ CFKAMIC C,qMPOSIT_S (NASA) IF_ p CSCL 14E -_°_ G3/38 02_6259 Prepared for the March Meeting of the American Society ........... _--_-_ for Nondestructive Testing https://ntrs.nasa.gov/search.jsp?R=19900014438 2020-01-20T11:42:17+00:00Z
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Page 1: Theory and ExperimentalTechnique for NOndestrdctive Evaluation Of … · 2013-08-30 · front reflection coefficient, ri figure 4. - uncertainty in attenuation as function of front

NASA Te_caI Mem0mndum 102561

T

Theory and ExperimentalTechniquefor _NOndestrdctive Evaluation_Of ................

CeramicComposi_es _ - - i

.... (NASA-TM-IO?56,1) THEORY AN_ EXP_-RTMt:NTAL N _0-23"/54 i_._:.-_>_5_"'_'-_:

TEC_4NTL_/IE FOR NqNDEST_UCTIVF- EVALUATIq_N GF __Z__ ___

CFKAMIC C,qMPOSIT_S (NASA) IF_ p CSCL 14E -_°_

G3/38 02_6259

Prepared for the

March Meeting of the American Society

........... _--_-_for Nondestructive Testing

https://ntrs.nasa.gov/search.jsp?R=19900014438 2020-01-20T11:42:17+00:00Z

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Page 3: Theory and ExperimentalTechnique for NOndestrdctive Evaluation Of … · 2013-08-30 · front reflection coefficient, ri figure 4. - uncertainty in attenuation as function of front

THEORY AND EXPERIMENTAL TECHNIQUE FOR NONDESTRUCTIVE

EVALUATION OF CERAMIC COMPOSITES

Edward R. Generazlo

Natlonal Aeronautics and Space Administration

Lewls Research Center

Cleveland, Ohlo 44135

SUMMARY

The important ultrasonic scattering mechanlsms for SIC and SI3N 4 ceramlc

composites have been identified by examlnlng the interaction of ultrasoundwlth Indlvldual fibers, pores, and gralns. The dominant scattering mechanisms

have been identified as asymmetric refractive scattering due to porosity gradi-

ents In the matrix material, and symmetric diffractive scattering at the fiber-

to-matrix Interface and at indlvldual pores. The effect of the ultrasonicreflection coefficient and surface roughness on the ultrasonic evaluation has

been highlighted. A new nonintrusive ultrasonic evaluation technique, the

angular power spectrum scan (APSS), has been presented that is sensltive tomIcrostructural variations In composites. Preliminary results Indicate that

the APSS wlll yleld informatlon on the composlte mlcrostructure that Is not

available by any other nondestructlve technique.

CO

LOL_

INTRODUCTION

Advanced hlgh-temperature ceramics (ref. 1) are belng developed for usein the next generatlon of aerospace systems. Recently, considerable attentlon

has been glven to monolithic SIC and Si3N 4 (ref. 2) for these hlgh-temperature

applications. Research on monolithic ceramics subsequently led to the current

developmental research on advanced hlgh-temperature ceramlc composltes. These

composites consist of particles, whiskers, or flbers In ceramic matrices. A

variety of processlng techniques are being investigated in an effort to produce

h_gh-temperature composites wlth optlmlzed thermal and mechanical propertles.Plasma spraying, reaction bonding, slurry presslng, and slnterlng are typical

technlques used to produce hlgh-temperature ceramics. These processes often

result in a composite that has a wide varlablllty in mlcrostructure. Typi-

cally, mIcrostructural variations such as poroslty, agglomerates, graln size,Interracial structure between phases, and orlentatlon of phases all play a

role In determining the materials properties. The importance and effects ofthese and other mlcrostructural varlatlons on the composite materlals' thermal

and mechanical properties are being aggresslvely researched (refs. l to 8).

Ultrasonic C-scans and conventional x-ray radiography are routinely per-

formed for nondestructive evaluation of a variety of materials. These NDE

techniques reveal macroscopic internal features such as delamlnatlons, debonds,

porosity, and cracks. Each of these features is important when consideringthe use of the tested material where strength and Integrlty must be assured.

However, standard ultrasonic C-scans and conventional x-ray radiography cannot

be expected to characterize the crucial mlnute variations in the ceramicmlcrostructure that affect strength and toughness. For example, the character-

Izatlon of toughness llmltlng matrix-second phase interface is beyond the capa-blllty of these standard technlques. Advanced NDE technologies can be expected

_L

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to nonlntruslvely evaluate the second phase to matrix Interface in composites.

The goal of this work Is to move NDE technologles In the direction required

for asslstlng in the development of advanced ceramics. The prellmlnary resultsshown here Indlcate that an advanced ultrasonlc scannlng technique and analysls

w111 be required for these composlte systems. A new nonlntruslve ultrasonlc

evaluatlon technlque called the angular power spectrum scan (APSS) isdiscussed.

APS

APSS

Af

Ao

a

a I

BCS

B1,2,3

d

FS

Io

J

N

PASS

P

Rb

Rf

r

S

S/N

X

X'

SYMBOLS

angular power spectrum

angular power spectrum scan

flnal amplltude

ultrasonic wave of known amplltude

dlstance between adjacent fiber edges

pore diameter

buffer rod-couplant-sample

back surface echoes

distance between fiber centers

front surface

Intenslty at x : 0 or r . 0

Bessel function

number of flbers

preclslon acoustlc scannlng system

degree of fiber opacity

back reflection coefflclent

front reflection coefflclent

radial distance from beam axis on the image plane

complex wave speed

slgnal-to-nolse ratlo of the input ultrasonlc pulse

sample thickness

dlstance perpendicular to fiber axis on the image plane

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Z

O

e I

(_

¢

distance between pore, or f|ber, and the Image plane

measured attenuation

polar angle

angle of Incldence

wavelength

variance

uncertainty In attenuatlon measurement

azlmuthal angle

Subscrlpts

L Incident wave

m medlum through whlch wave propagates

IL longltudlnal Incldent wave

In long|tudlnal wave propagatlon

2L shear Incldent wave

2n shear wave propagation

BACKGROUND

Ultrasonlc Imaglng can be done by means of several technlques. The mostcommon Is the one used by commerclally available ultrasonic ImmerslonC-scannlng systems. An ultrasonic wave of known amplltude Ao Is transmlttedthrough a sample as shown in figure I. The final amplitude Af, or C-scanImage, Is a representatlon of relative attenuatlon, or energy lost, by theultrasonic wave as it traverses through the sample. Unfortunately, C-scanImages are not true representations of the energy lost by the ultrasonic waveas It travels through the sample. The ultrasonic reflectlon coefficients atthe water-to-sample Interfaces are not generally imaged. These reflectloncoefflclents are large and must be Included in the analysls for determlnatlonof the attenuation. The reflection coefflclent |s used to determine the accu-

racy of an acoustic Image. It can also be used to determine the most accurateacoustlc Imaging technique to use.

In order to obtaln the reflectlon coefflclent at the back surface, a modl-

fied two-transducer arrangement must be used (fig. 2) where the transducersare both transmitters and receivers. The variance o_ In the attenuatlon

measurement for thls Immersion arrangement Is given by reference 9

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TRANSMITTER

H20

/"- SAMPLE1

Af

H20

RECEIVER

FIGURE 1. - STANDARD IMMERSION ULTRASONIC C-SCANNING ARRANGE/'WZNT.

ITRANSMITTER/

RECEIVER

H20

i

.,.--SAMPLEI

H20

TRANSMITTER/

RECEIVER

FIGURE 2. - MODIFIED IMMERSION ULTRASONIC SCANNING ARRANGEMENT NEEDED TO

DETERMINE REFLECTION COEFFICIENTS AT FRONT AND BACK SURFACES. ULTRASONIC

WAVE OF KNOWN _LITUDE, AO; FINAL AMPLITUDE, Af.

4

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,b)[(,.R,).4,_]ac_ s l (l- 22 22 (I_,_)2[(,.,_).4,_]

+

,,)(iR0)I 22 22

+

2(._R_)(.•,_)e2°X.,)(IRb)1 - 22 - 22

112

(1)

where SIN Is the slgnal-to-nolse ratlo of the Input ultrasonic pulse, a Is

the measured attenuation, Rf and Rb are the reflection coefficient magni-tudes on the Front and back surface of the sample, respectively, and x Is

the sample thickness.

Ceramics generally have immersion reflection coefficients of about 0.92.

Thls corresponds to an uncertalnty of about 15 to 30 percent. If we are to

understand the interaction of ultrasonic waves wlth ceramics systems, we need

the most accurate evaluation technique available.

An alternatlve technlque to immerslon scanning Is contact scannlng. This

technlque uses a precision acoustic scanning system (PASS) that Is describedIn detail elsewhere (refs. 10 to 13). Briefly, a single transducer is used to

make precise and accurate attenuatlon measurements. The experimental arrange-ment for contact ultrasonic measurements Is shown In flgure 3. An ultrasonlc

wave Is Introduced Into the sample vla the buffer rod-couplant-sample (BCS)

interface. The ultrasonlc wave subsequently echoes within the sample. By

measurlng the reflection coefficient

%-BACK SURFACE

X rB 1'\_,

J SPECIMEN

FRONT / / l ISURFACE---/ /

QUARTZ

BUFFER

ROD

i/

PIEZO- //

ELECTRIC /CRYSTAL--/

rB2'

IBi'FS 1, FS2

TO PULSER-

RECEIVER

Rf (ref. 12) at the BCS Interface and

Ik.___ _

TIME

FIGURE 3. - CONFIGURATION FOR CONTACTULTRASONIC MEASUREMENTS.

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the approprlate echoes, the ultrasonic attenuation can be determined.

lance In the attenuation measurement for thls arrangement Is glven byreference 12:

The var-

_2R2 ]

S I [Kfb e4_X] e4_x+ 4 22 1

1/2

(2)

Note that the sample need not be alr-backed. That Is, Rb may be <I. Ceramics

generally have contact reflection coefficients of about 0.5. Thls corresponds

to a variance of about 7 to 15 percent.

Equatlons (I) and (2) are graphically shown In figure 4. The configura-tion havlng the lowest varlance values obta|ned from equations (1) and (2) Is

shown. The solid line In the f|gure can be used to make a decision about which

technlque should be applied for a partlcular experimental sample. Above the

solld line, a precision contact pulse-echo measurement is preferred. Below

the solld llne, an Immerslon through transmlsslon yields the least uncertalntyIn the attenuatlon measurement.

1.0

r2.75 < O'K_ 3.25I

i -3.75 < O'i CONTACT PULSE-ECHOI I r-

i_ _] r3.25< o'_<3,75 i]! I I

.9

.8

z .7hl

_. .6tl

L_J

U. ,3L_r,-

.I

0 .I .2 .3 .4 .5 .6 .7 .8 .9 1.0

FRONT REFLECTION COEFFICIENT, RI

FIGURE 4. - UNCERTAINTY IN ATTENUATION AS FUNCTION OF

FRONT AND BACK SURFACE REFLECTION COEFFICIENTS FOR

BOTH IMMERSION AND CONTACT ULTRASONIC SCANNING. CON-

TACT SCANNING METHOD IS MORE ACCURATE ABOVE THE SOLID

LINE. LONG-DASHED LINE INDICATES THE UNCERTAINTY FOR

THE IMMERSION ARRANGEMENT WHERE THE SAMPLE HAS IDENTI-

CAL REFLECTION COEFFICIENTS ON BOTH SIDES. HERE 20X =

I, 0 = I, AND O' = LOG [O0/O(S/N)].

6

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Immersion ultrasonic systems generally have similar reflectlon coeffl-

clents for Rf and Rb. The variance Is symmetric wlth respect to the Rf = Rbaxls for Immersion measurements. The long dashed llne In figure 4 Indicates

the path used to determine the variance. The stated reflection coefficients

are for acoustically flat (i.e., flat when compared with the ultrasonic wave-

length) specimens. Any additional roughness will further increase the reflec-

tion coefficient. Many solid materlals wi11 flt on thls curve between 0.84 and0.97.

Figure 5 shows the varlance for PMMA, PMC, AI, Pb, SlC, AI302, NI, W, and

SI3N 4 for both immersion (Rf = Rb) and contact ultrasonic methods. When evalu-

ating NI, SiC, SI3N 4, AI302, and W, the contact pulse-echo method yields theleast uncertain and most accurate attenuation measurement. Therefore, contact

scanning should be, and Is, used here for evaluating the monollthlc ceramicmatrix material.

10

8

64

2

C) PMMA

[:7 PMC

E) AI

0 Pb

SiC

o Ab02<> Ni

%7 W

0 Si3N4

-- CONTACT CASE

.... IMMERSION CASE

----- MINIM_ UNCERTAINTY

-- rn AT,,,,/- RNT,..,C_I) . VALUE FROMCONTACT |

B - METHOD e

-- IMMERSION (Rf = RB) _\,,. ..............

.........F I° " I I I.2 .ll .6 ,8 1.0

REFLECTION COEFFICIENT, RS

FIGURE 5. - UNCERTAINTY COMPARISONFOR SEVERAL MATERIALS. FOR AI302,

Ni, W, SiC, AND Si3N 4 THE UNCERTAINTY IS LOWERWHENUSING A CONTACTSCANNING METHOD. THE CURVESARE GENERATEDFROMEOUATIONS 1 AND 2.

THE DASHEDLINE IS FOR THE IMMERSION CASE. THE SOLID LINE IS FOR

THE CONTACT CASE. THE DASHED-DOI-II_DLINE INDICATES THE MINIMUM UN-

CERTAINLY"VAL_ THAT THE CONTACT METHOD CAN YIELD. HERE 2aX = I,

o = 1, AND o' = LOG [Oa/O(S/N)].

APPROACH

Ultrasonic evaluation of composltes may be approached from two directions.

The complete composite system can be interrogated as a whole system. Theresultant ultrasonic signals are complicated and difficult to interpret. Since

the actual mechanisms that are forming these signals remaln unknown, their

interpretation is subject to question. An alternatlve to this approach Is toexpllcltly determine the Interaction of ultrasound wlth each Indlvldual

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component, or phase, of the composlte. Thls Informatlon Is then used for for-mulatlng theories that explaln the ultrasonlc slgnals obtained from the fullcomposite system. The latter approach is used for thls work.

SCATTERING DUE TO GRAIN BOUNDARIES

The matrix materials SiC and SI3N 4 are acoustically slmllar; that Is,

they have similar but not identical densities, ultrasonlc velocities, ultra-sonic attenuation, and elastic modull (see table I). The ultrasonic attenua-

tlon (for frequencies below 50 MHz) due to grain boundary scattering has been

found to be negllglble for nearly fully dense SIC and SI3N 4 having grain sizes

less than 15 Nm (refs. II and 12). Therefore, grain boundary scattering need

not be considered for SIC and $13N 4 matrix materla1.

Materlal

SiC

SI3N4

Density,

glcc

3.12

3.28

TABLE I

Young'smodulus,

GPa

440

310

Velocity,

cm/_sec

1.22

1.09

Attenuatlon,

Nlcm,50 MHz

<0.I<0.1

SCATTERING DUE TO PORES

The Interaction of ultrasonic waves with Individual pores is well under-

stood. When an ultrasonic wave interacts with a pore, a spherical wave Is

generated at the pore site. The spherical wave interacts with the maln beam toform a diffraction pattern. The Intensity observed at the plane perpendlcular

to the sound direction Is given by the relation (ref. 14)

(3)

where Jl is the Bessel functlon, a' Is the pore diameter, z is the distancebetween the pore and the Image plane, r is the radial distance from the beam

axis on the image plane, and Io Is the intensity at r - O.

The spherical wave and diffraction pattern are observable by many ultra-sonic Imaging techniques. The ultrasonic surface wave and longitudinal wave

images in figure 6 reveal the spherical wave and spherical diffraction pattern,

respectively, from a single subsurface pore. The ultrasonic energy is symmet-

rically scattered to form a cylindrically symmetric pattern on a plane perpen-dicular to the beam axis.

A composlte generally has many pores dlspersed throughout the matrix.

The energy scattered from these pores is not observable as Individual ring pat-terns. The patterns overlap and form a uniform cylindrically symmetrlc inten-

sity background. Increasing the number of pores (with the same dlameter) perunlt volume will result in an increased amount of scattering per unit volume

8

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ORIGINAL PAGE

BLACK ARD _/.H_JI_P_HOIOGRAP_H

(a) SURFACE WAVE IMAGE RE-VEALING SUBSURFACEPORE IN

SiC.

(b) SCANNING LASER ACOUSTIC MICROSCOPE

IMAGE REVEALING A SUBSURFACEPORE IN

SiO 2. ONLY THE RIGHT HALF OF THEDIFFRACTION PATTERN IS VISIBLE BE-

CAUSE OF THE EXPERIMENTAL CONFiGURA-TION.

FIGURE 6. - ULTRASONIC IMAGES OF SUBSURFACEPORES,

and, therefore, a decrease In tntensltles. It is noted here that partially orIncompletely bonded regions between composite lamina are ultrasonically equiva-lent to reglons of increased porosity. Therefore, a cylindrically symmetricdecrease In intensity can be due to increased matrix porosity or incompleteInterlaminar bonding.

SCATTERING DUE TO POROSITY GRADIENTS

Refraction of waves occurs at boundaries that are veloclty mismatched.

For planar boundaries between elastic media (e.g., the boundary betweenmedium I and medium 2), longitudinal and shear waves are refracted and

reflected at the boundary at an angle determined by the well-known Snell'slaw for elastic media (ref. 15):

FSmn],,nsln *Lmn LSlL]

(4)

where e' and _ are the angles measured from the surface normal vector (e'is also the Incident angle), and S Is the complex wave speed. The sub-

script L corresponds to longitudinal (L = 1) or shear (L - 2) incident

wave. The subscript m Indicates which medium, l or 2, the wave is propagat-

ing through. The subscrlpt n denotes longitudinal (n - l) or shear (n = 2)

wave propagation.

The ultrasonic velocity and attenuation images for a specimen of SlC are

shown in figure 7. The ultrasonic velocity In porous media is linearly related

to the density (ref. 16). The high velocity region in the upper left of the

figure corresponds to a high density region. The hlgh attenuation band In the

attenuation Image is of particular interest. This high attenuation band occursat the density gradient boundary existing between hlgh and low density reglons.

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ORIGINAL PAGE

BLACKA/ D .VV_HI] PJ!O_T.OGRA£Ji

CM/pSEC

Np/CM

.99 1.04 1,09t I : I

1.111J

1

(a) VELOCITY IMAGE. (b) ATTENUATION IMAGE.

FIGURE 7. - ULTRASONIC VELOCITY AND ATTENUATION IMAGES FOR SiC OBTAINED BY

PRECISION ACOUSTIC SCANNING SYSTEM (PASS).

The velocity gradlents yield hlgh attenuation due to refractive scatter-Ing at thls boundary. That Is, the acoustic energy Is belng redirected,

because of refraction and reflection, from the maln acoustic beam. Therefore,

regions of hlgh attenuation may Indicate the presence of density gradlents and

not necessarily flaws. Refractive scattering Is, In general, asymmetric wlth

respect to the Inltla] direction, or beam axis; that is, If energy Is refrac-

tively scattered off at an angle +_, then energy wll] not, simultaneously, be

scattered off at the symmetric angle -_.

SCATTERING DUE TO FIBERS

The interaction of ultrasound with continuous fibers Is analogous to theinteraction of light wlth silt-shaped apertures. The Intenslty of the scat-

tered wave from a set of parallel fibers embedded In a matrix Is given byreference 17,

I = O[ 6_ _ _in2 Y j_a _d sin c - -- (5)B = E" sin ¢, Y = X _ - tan 1 zX'

where z Is the distance between the fiber and the image plane, x' Is the

distance perpendicu|ar to the fiber axls on the Image plane, a Is the distance

between adjacent fiber edges, d Is the distance between fiber centers, N Is

the number of fibers, and Io Is the intensity at x - O. Here it Is assumed

that the fibers are acoustically opaque. The wave Is transmltted through the

lO

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grating vla the matrix material between adjacent fibers. If we let N = 1then we have the solution for a single fiber in a matrix.

If the flbers are not acoustically opaque, then the Intenslty observed has

two components. One component is caused by a unlform background (e.g., letthe flbers be constructed of material Identlcal to the matrix, and perfectly

bonded to the matrlx). The other component Is caused by a grating (eq. (5))

where the maximum Intenslty of the dlffractlve component Io Is replaced by

pIo. The degree of opaclty of the fibers p varles between fully opaque

(p : l) and fully transmitting (p = 0).

The opacity of the flbers embedded In a matrlx material Is determined by

both the fiber materlal and the degree of bondlng between the flber and the

matrix. For example, If the fiber and the matrlx are both of the same mate-

rlal and the fiber Is perfectly bonded, then p - 0 so that no dlffractlon

w111 occur. If the same flber Is completely dlsbonded from the matrix, then

p , l and dlffractlon wlll occur to yield the maximum posslble intensity of

the dlffractlve component, Io. Alternatlvely, if the flber material Is differ-ent from that of the matrlx and Is perfectly bonded, then the opacity w111

always be greater than zero and less than one. That is, dlffractlve scatterlng

wlll always occur. A completely dlsbonded flber, p : l, w111 have identicalresults whether the fiber materlal Is slmllar or dissimilar to the matrlx

material.

In order to evaluate the Interactlon of ultrasound wlth flbers embedded

In a matrix materlal, a single fiber composite system is used. Figure 8 shows

an ultrasonic backscattered image of a single surface-breaklng SIC fiber in a

$13N 4 matrix. The fiber is 1.5 cm long and 140 _m In diameter. In the upper

ORIGINAL PAGE

B I.ACK AND WHLTF I?}_OIOGRAP_H

FIGURE8. - BACKSCATTEREDDIFFRAC-

TION PATTERNFROM SINGLESiC

FIBER (1.5cm LONG, 140 pm DIAM)

EMBEDDED IN A Sign4 MATRIX.

II

ORIGINAL PAGE

BLACK AND WHITE PHOTOGRAPH

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part of the figure, the fiber is exposed to the surface and does not show anydiffraction effects. The flber Is subsurface in the lower part of the Figureand exhibits a strong diffraction effect analogous to an optlcal single-slitdlffractlon pattern. The diffraction pattern is symmetric with respect to thefiber axis. The two dark circular areas at the ends of the fiber are regions

of mlcrocracklng and porosity that formed during the stntertng process. Thelower subsurface crack zone exhibits a circularly symmetric diffraction pat-tern slmtlar to that found for subsurface pores (fig. 6).

SUMMARY OF SCATTERING MECHANISMS

The domlnant scatterlng mechanlsms for ceramic composltes are:

(1) Symmetric diffractive scattering at Indlvldual pores

(2) Symmetrlc diffractive scatterlng at fibers

(3) Asymmetric refractive scattering at density gradients

Grain boundary scattering has been found to be negllgible. The above 11st ofultrasonic scattering mechanisms can be used to Identlfy an ultrasonic tech-

nlque for evaluating ceramic composites. The key factor in the above list Is

the symmetry of the scattered energy. Thls factor Is the main guide In devel-

oplng an appropriate ultrasonic evaluation technique for ceramic composites.

ANGULAR POWER SPECTRUM

The angular (polar) power spectrum (APS) of the wave transmitted through

a composite wlll contaln all the Informatlon on each of the above scattering

mechanisms. One posslblearrangement for det_rmlnlng the angular power spec-

trum is shown In figure 9(a). The angular power spectrum Is obtained at a

point by moving the receiver, at a fixed radii, over the half-space containingthe transmltted signal. Here the incident wave Is transmitted and scattered

by the presence of the composite specimen. A receiving transducer Is scanned

in an angular fashion to determine the energy scattered In the hemisphere

described by -90 ° _ e _ 90° and 0 _ ¢ < 180°. Thls may also be done with

elther a planar or nonplanar array of transducers or a slngle or multlpietranducer(s) rotated about the e and ¢ axes. Many other rotation and array

design combinations may be used to determine the APS. The mlcrostructure of

the composites varles through the bulk of the specimen; therefore, a scanning

arrangement wll] be required to obtain a complete APSS of the specimen.

Asymmetric components In the APS are indications of porosity or densitygradients. The presence of continuous fibers in multldlrectlonal composites

wlli yield power spectrums that are symmetric with respect to the fiber axes.

If there are N uniformly spaced fiber directions perpendicular to the inci-

dent sound, then the power spectrum will be 2N-fold symmetrlc with respect tothe Incldent sound direction. The width of the spectrum Is a function of

angle, ¢, and is affected by the poroslty_the number of flber layers, thefiber diameter, the distance between the fibers, and the degree of bonding

between the flber and the matrix. The amplitude of the spectrum along themain beam axls indicates the total amount of energy scattered out of the maln

beam due to all of the above mechanisms.

12

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SOLID ANGLE SCAN RECEIVER

/

CO_OS ITEm/

(a) ORIENTATION AND PLACEMENT OF TRANSDUCERS AND SA/_PLE

TO DETERMINE THE APS.

._ REFRACTIVE SCATTERING/ F AT POROSITY

[_'_/ I GRADIENTSL,.,

CONSTANT POWER ..i'"CONTOURS --I

(b) CONSTANT POWER CONTOURS OF APS.

POWER

i \

8 7r

2 2

(c) PARTIAL APS (APS AT

CONSTANT ANGLE. ® = 0).

FIGURE 9. - ANGULAR POWER SPECTRUM (APS) OF WAVE TRANSMITTED THROUGH A

COMPOSTTE,

The interpretation of the APS Is best described by examples. Assume that,for a particular composite system, the fiber diameters are uniform, the fiber

spacings are uniformly repetitive, and the fiber-to-matrix bond is uniform

everywhere. An APS constant power contour level for a 0°/90 ° composite system

should appear as shown in figure 9(b). Thls APS Is four-fold symmetric wlth

respect to the beam axis. A uniform increase (or decrease) in porositythroughout the sample will Increase (or decrease) the diameter D of the cir-

cularly symmetric constant power component of the APS (figs. 9(b) and (c)).

If the bonding between the matrix and the fiber Is weakened (p - 1) then the

amplitude of the four-fold symmetrlc diffraction pattern wlll increase. If

there are poros|ty gradients present, the component of the APS due to porosity

will form an asymmetric shape as shown In the dotted curve In f_gure 9(b).

PRELIMINARY EXPERIMENTAL RESULTS

Two Identlcally produced SIC/SiC laminates wlth 0o/90 ° Nicalon fabric com-

posites were used. Conventional radlographlc and ultrasonic C-scan Images areshown In flgure lO for speclmens labeled A and B. The two radlographlc images

appear slmIIar. Systematic variations In density are observed in both speci-

mens as a series of O.5-cm-dlam dark disks spaced about 1.5 cm apart. These

dark regions correspond to high density regions. The fiber weave pattern can

also be observed in radiographs.

13

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Ultrasonic C-scans at lO MHz(flg. I0) reveal quite different results.

The ultrasonic image of sample A is more uniform and darker (dark (light)

corresponds to poor (good) ultrasonic transmission) than that of sample B.

This Indicates poor InterIamlnar bonding In sample A. A very porous system

could also produce thls type of image. However, the radiographs indicate that

the porosity for the two specimens Is similar. The ultrasonic image for speci-

men B has a large amount of fluctuations in the Intensity and has the appear-

ance of being blurred.

t_

lcm

X-RAY IMAGE ULTRASONIC IMAGE

FIGURE 10. - RADIOGRAPHIC AND ULTRASONIC C-SCAN IMAGES.

2X

A complete APSS system has not yet been developed. In lleu of this, a

partial APS was done at IO MHz by holding one angle constant (¢ = 0°) and

-60 ° < e _ 60°. Figure If(a) shows the APS without the sample present. The

symmetry of the signal Indicates that the transmltter and receiver have rela-

tively symmetric responses. The partial APS at the points labeled P on speci-

mens A and B are shown in figures 11(b) and (c), respectlvely. The APS's arenormalized to have a maximum amplitude of one. The APS for specimen A Is rela-

tively symmetric and Indicates that thls region Is relatively free of porosity

gradients. In contrast, the APS for specimen B Is asymmetric and indicates

the presence of poroslty gradients. These gradients may be due to variationsIn the Interlamlnar bond at this point.

_GOo 0o 60°

O

(a) SIGNAL WIIIIOUT SPECIMENS.

_600 0o 60o

(b) SPECIMEN A: ALMOST SYMMETRIC AT

_GOo 0o GO°

(c) SPECIMEN B: ASYI_tETRICAT POINT P.

POINT P.

FIGURE 11. - PARTIAL ANGULAR POWER SPECTRUM (® = O) FOR WOVEN COMPOSITES.

(POINT P IS SHOWN IN FIG. 10.)

14

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A quas1-APSwas done by letting @= 0°, -60 ° _ e < 60° , and moving thereceiving transducer along a llne parallel to the speclmen surface and along

the e-axis of rotation. The resulting Images are shown In figure 12. Fig-

ures 12(a) to (c) are quasl-APS images wlthout the sample present, and for

speclmens A and B, respectively. A visual comparison between flgures ll(b)and (c) dramatlcally reveals the presence and effect of asymmetric scatterlng

detected by the APS technique.

(a) SIGNALWITHOUTSPECIMEN.

(b) ALMOSTSYMMETRICAT POINT P FOR SPECIMENA.

-600 60o

(c) ASYMMETRICAT POINT P FOR SPECIMENB.

FIGURE 12. - QUASI-APS(ANGULARPOWER SPECTRUMWITH® = O) FOR WOVEN COM-

POSIES. (POINTP IS SHOWN IN FIG. 10.)

I °

°

3.

.

.

,

o

REFERENCES

HITEMP Review 1989: Advanced High Temperature Engine Materlals Technology

Program. NASA CP-IO039, 1989.

Structural Ceramics. NASA CP-2427, 1986.

Grell, P.; Petzow, G.; and Tanaka, H.: Sinterlng and HIPplng of S111conNltrlde-S111con Carbide Composite Materlals. Ceram. Int., vol. 13,

no. l, 1987, pp. 19-25.

Nlckel, K.G.; et al.: Thermodynamic Calculations for the Formation of

SlC-Hhlsker-Relnforced $13N 4 Ceramics. Adv. Ceram. Mater., vol. 3,

no. 6, Nov. 1988, pp. 557-562.

Freemann, M.R.; Klser, J.D.; and Sanders, W.A." A Slnterlng Model for

SlCw/SI3N4 Composites. NASA TM-I01336, 1988.

Wel, G.C.; and Becher, P.F." Development of SiC-Whisker-Relnforced Ceram-Ics. Am. Ceram. S,c. Bu11., vo1. 64, no. 2, Feb. 1985, pp. 298-304.

Kobayashl, S.; Kandorl, T.; and Wada, S.: M1crostructure of SI3N 4 Compos-Ites Reinforced with SiC Whlskers. J. Ceram. S.c. Jpn., vol. 94, no. 8,

1986, pp. 903-905.

15

Page 18: Theory and ExperimentalTechnique for NOndestrdctive Evaluation Of … · 2013-08-30 · front reflection coefficient, ri figure 4. - uncertainty in attenuation as function of front

.

.

I0.

II.

12.

13.

14.

15.

16.

Ishlgakl, H.; et al.: Trlbologlca] Properties of SIC Whlsker Contalnlng

S|11con NItrlde Composite. J. Trlbology, vol. II0, no. 3, July 19BB,pp. 434-438.

17.

Generazlo, E.R.; and Roth, D.J.: Recent Advances In Nondestructive Evalu-

atlon Made Possible by Novel Uses of Video Systems. MlCon 90: Advances

In Video Technology for Mlcrostructural Control, ASTM STP-I094, George

Van der V(x)rt, ed., American Society for Testing and Materials, PhIIadel-

phla, May 23, 1990. (Also, NASA TM-I02491).

Generazlo, E.R.; Roth, D.O.; and Stang, D.B.:

Porosity Variations Produced During Slnterlng,vo1. 72, no. 7, July 1989, pp. 1282-1285.

Ultrasonic Imaging ofJ. Am. Ceram. Soc.,

Generazlo, E.R.; Roth, D.J.; and BaakIInl, G.Y.: Acoustic Imaging of,

Subtle Porosity Variations in Ceramics. Mater. Eval., vol. 46, no. lO,

Sept. 1988, pp. 1338-1343.

Generazlo, E.R.: The Role of the Reflection Coefficient in Preclslon

Measurement of Ultrasonic Attenuatlon. Mater. Eval., vo1. 43, no. 8,

July 1985, pp. 995-I004.

Generazlo, E.R.; Stang, D.B.; and Roth, D.J.: Interfaclng Laboratory

Instruments to Multluser, Virtual Memory Computers. Proceedings of The

Sixteenth Annual Review of Progress In Quantltatlve Nondestructive Evalua-

tion, vol. 9, D.O. Thompson and D.E. Chlmentl, eds., Plenum Press,

May 1990, pp. I079-I085. (Also, NASA TM-4106).

Chou, C.H.; Khurl-Yakub, B.T.; and K1no, G.S.: Transmlsslon Imaging: For-

ward Scattering and Scatter Reconstructing. Acoustical Imaging, vol. 9,

Vlsuallzatlon and Characterization, K.Y. Wang, ed., Plenum Press, 19BO,

pp. 357-377.

Cooper, H.F., Jr.: Reflectlon and Transmission of Obllque Plane Waves ata Plane Interface Between Viscoelastic Media. J. Acoust. Soc. Am.,

vol. 42, no. 5, 1967, pp. I064-I069.

Roth, D.J., et a1.: Review and Statlstical Analysis of the UltrasonicVelocityMethod for Estimating the Porosity Fraction In Polycrystalllne

Materials. NASA TM-10250_, 1990.

3enklns, F.A.; and White, H.E.: Fundamentals of Physical Optics.

McGraw-HIll, 1937, Chapter 7.

16

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Report Documentation PageNationalAeronauticsandSpace Administration

1. Report No, 2. Government Accession No. 3. Recipient's Catalog No.

NASA TM- 102561

5. Report Date4. Title and Subtitle

Theory and Experimental Technique for Nondestructive

Evaluation of Ceramic Composites

7. Author(s)

Edward R. Generazio

9. Performing Organization Name and Address

National Aeronautics and Space AdministrationLewis Research Center

Cleveland, Ohio 44135-3191

12. Sponsoring Agency Name and Address

National Aeronautics and Space Administration

Washington, D.C. 20546-0001

6. Performing Organization Code

8. Performing Organization Report No.

E-5381

10. Work Unit No.

510-0 I-0A

t 1. Contract or Grant No.

13. Type of Report and Period Covered

Technical Memorandum

14. Sponsoring Agency Cede

15. Supplementary Notes

Prepared for the March Meeting of the American Society for Nondestructive Testing, Columbus, Ohio,

March 15, 1990. Invited paper.

16. Abstract

The important ultrasonic scattering mechanisms for SiC and Si3N 4 ceramic composites have been identified by

examining the interaction of ultrasound with individua[ fibers, pores, and grains. The dominant scattering mech-anisms have been identified as asymmetric refractive scattering due to porosity gradients in the matrix material,

and symmetric diffractive scattering at the fiber-to-matrix interface and at individual pores. The effect of theultrasonic reflection coefficient and surface roughness on the ultrasonic evaluation has been highlighted. A new

nonintrusive ultrasonic evaluation technique, angular power spectrum scanning (APSS), has been presented that is

sensitive to microstructural variations in composites. Preliminary results indicate that APSS will yield information

on the composite microstructure that is not available by any other nondestructive technique.

17. Key Words (Suggested by Author(s))

Composites; Nondestructive evaluation; Ceramics;

Ultrasonics; Porosity; Microstructure; NDE; NDT

18. Distribution Statement

Unclassified- Unlimited

Subject Category 38

19. Security Clsssif. (of this report) 20. Security Classlf. (of this page) 21. No. of pages

Unclassified Unclassified 18

NASAFORUls2e OCTM*For sale by the National Technical InformationService, Springfield,Virginia22161

22. Price"

A03

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