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
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
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
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
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
,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.
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
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
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
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.
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
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
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
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
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
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
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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
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tion, vol. 9, D.O. Thompson and D.E. Chlmentl, eds., Plenum Press,
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ward Scattering and Scatter Reconstructing. Acoustical Imaging, vol. 9,
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16
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
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