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High-Reliability Joiningof CeramictoMetal

HOWARDMIZUHARA,'E. HUEBEL, and T. OYAMA


WESGODivision, GTEProduct Corporation, Belmont, California94002
W
ith the development of new ceramic
materials, including those for struc-
tural applications, there is an increasing
demand to join ceramic components to
metal structures. The most commonly used
methodis themoly-manganyseprocess. 1-3
This process is well-established and pro-
duces highly reliable joints between ce-
ramics and metals. However, the moly-
manganese process requires two process-
ing steps: metalization of the ceramic, fol-
lowed by brazing. It is, therefore, time-
consuming. Furthermore, the metaliza-
tion process is conducted at very high
temperature ( -1500C). In addition, joint
properties are sensitive to process varia-
bles, and, hence, precise process control
is required to obtain the reliable joints.
As a result, this process is very expensive.
Direct brazing between ceramic and
metal is also possible through active filler
metals.4-'o Because this is a one-step pro-
cess, it is simple and economical. Al-
though active metal brazing has been in-
vestigated since 1940, it has not been
widely accepted because of inconsistent
joint properties. There are several meth-
ods of the active metal brazing. For ex-
ample, one method involves a sheet of ti-
tanium (the most commonly used active
element) that can be cladded by two sheets
of the conventional brazing metals.6 An-
other example usestitanium hydride pow-
ders mixed with powders of conventional
brazing metals.s However, the most eco-
nomical method utilizes afiller metal where
an active element(s) forms a true alloy
with the base filler metal. The present
investigation centers on a copper-silver
filler metal containing titanium as an ac-
tive element (Cusil-ABA)@. * The nominal
chemical compositions and several im-
portant properties of the Cusil-ABA@ are
listed in Table 1. Because the concentra-
tion of the titanium is relatively low (2
wt%), titanium dissolves in the matrix
(mainly copper-rich phase) as a solid so-
lution.
There are a variety of different prop-
erties to be considered in the ceramic-
metal joints, e.g., mechanical, electrical,
thermal properties, etc. Depending on the
application of the joint, some properties
are more important than others. However,
'Member, American Ceramic Society.
'GTE Product Corp., WESGO Division, Belmont,
CA.
Table I. Chemical Compositions and Properties of Cusil-ABNMFillerMetal
Nominal composition 63 wt% Ag+35 wt% Cu+2 wt% Ti
Physical properties
815C (I 500F)
780C (l435F)
9.8 Mg.m-J (5.2 troz.in.-3)
180 W.m-I.K-1 (104 Btu.h-'.ft-,.oF-')
18.5 X 10-6 K-I (10.3 X 10-6 OF-I)
Liquidus temperature
Solidus temperature
Density
Thermal conductivity*
Thermal expansion coefficient (RT to 500C)
Electrical properties
44 x 10-9 Q.m
23 x 106 Q-I .m-I
Mechanical properties
83 GPa (12 x 106 psi)
0.36
271 MPa (39300 psi)
346 MPa (50200 psi)
20%
1100 MPa (110 KHN)
Electrical resistivity
Electrical conductivity
Young's modulus
Poisson's ratio'
Yield strength
Ultimate tensile strength
Elongation (2-in. gage section)
Hardness
'Calculated from the electrical conductivity by the Wiedmann-Franz law. 'Estimated by the volumetric
average of the Poisson's ratios for silver and copper.
the mechanical properties are some of the
most important properties for any joint.
Joints without any mechanical strength
can be regarded as unsuccessful joints. In
the present paper, therefore, the mechan-
ical properties of the joints are empha-
sized. For the evaluation of the joint prop-
erties, it is essential to establish proper
testing methods so that effects of the pro-
cessing variables can be detected accu-
rately and consistently. It is also desirable
that the results of the tests provide mean-
ingful engineering parameters for design
engineers.Severaltestingmethodsareex-
amined.The optimumtestingmethodsfor
the evaluation of the ceramic-metal joint
properties are recommended.
One of the major problems of joining
ceramic to metal is the thermal expansion
mismatch between them. Generally, the
ceramicmaterialshavelowerthermal ex-
pansioncoefficientsthan the metallicma-
terials. A list of the thermal expansion
coefficients of several structural ceramics
and common metals is given in Table II.
The difference in the thermal expansion
coefficients can lead to very high stress at
the brazed region during cooling from the
brazing temperature to room tempera-
ture. The high stress sometimes results in
joint failures or unreliable joints. There-
fore, the thermal stress problems should
be overcome to obtain reliable joints be-
tween the ceramic and the metal.
In the present paper, the active metal
brazing process of the ceramic to the metal
is examined in detail. Influences of all
process variables, including joining ma-
terials, engineering joint design, and braz-
ing procedures, are evaluated to obtain
reliable joints between ceramic and metal
with the active filler metal.
Joining Materials
Ceramic-metal brazing involves three
materials: ceramic, metal, and filler metal.
Properties of each material influence the
resultant joint properties.
Ceramic Component
The ceramic, because of its inherent
brittleness, is the most critical material
for obtaining reliable joints. The base
properties of the bulk ceramic member
are essential. When the properties of the
bulk ceramic are not sufficient, the ther-
mal stress simply fractures the ceramic
member. Furthermore, the surface con-
dition of the ceramic is also very impor-
tant for the joint reliability.7.'oMizuhara
and Mally7 and Mizuhara and Huebel'O
demonstrated that, when the ceramic sur-
face is in the as-ground condition, only
marginal joint properties between the ce-
ramic and the metal will be obtained.
When the ceramic material is ground
by a metal-bonded diamond wheel, mi-
crocracks are introduced at the surface
of the ceramic. The size of the micro-
cracks depends on the diamond grit size
of the wheel and also on the rate of ma-
terial removal. The surface damage can
initiate major cracks in the ceramic by
the thermal stress and, hence, result in an
unreliable joint. Therefore, the ceramic
surface should be free of damage to ob-
CERAMIC BULLETIN, VOL. 68, NO.9, 1989 (@ACerS)
1591 Reprinted for The American Ceramic Society Bulletin. Vol. 68, No.9, September 1989
Copyright @ 1989 by The American Ceramic Society, Inc.
tain high-reliability joints. This condition
can be met simply by using sintered ce-
ramic materials. However, nearly all sin-
tered ceramic parts over about 2 cm in
size should be ground, because distortion
of the parts during the sintering requires
grinding for dimensional control. Ground
ceramic materials should be treated fur-
ther to obtain a defect-free surface con-
dition. This can be performed by a resin-
tering or lapping process. In the resin-
tering process, the damaged layer is healed
through sintering. In the case of the lap-
ping process, the damaged layer is phys-
ically removed. It should be mentioned
that the thickness removed by the lapping
must completely eliminate the surface
damages. In the present investigation, AL-
995* (99.5% AlzOJ)is used as the ceramic
member of the joint. Two surface condi-
tions are examined: the as-ground and the
ground-and-resintered conditions. The re-
sintering process is conducted at 1650C
for 1 h.
Metal Component
The metal is generally ductile and,
hence, does not readily fracture. How-
ever, there are several important require-
ments to obtain reliable joints.
The metal should exhibit only low
blushing (or surface flow)of the filler metal.
The extensive blushing effectively de-
pletes the amount of the active element
available for wetting the ceramic. Among
the parameters controlling the blushing
behaviors are the relative properties of
the metal member and filler metal. Ef-
fects of the metal member on the blush-
ing behaviors are demonstrated in Fig. 1.
In these examples, the Cusil-ABA@foils
(50-tLmthick) are placed on different sub-
strate metals (and alumina) and melted
under vacuum at 830C. As demonstrat-
ed in Fig. 1, the Cusil-ABA@shows dif-
ferent blushing behaviors depending on
the substrate material. No blushing is ob-
served on alumina, 304 stainless steel, or
copper, whereas extensive blushing is ob-
served on nickel. These results demon-
strate that the blushing of the filler metal
can be minimized by proper selection of
the metal member. Another method to
eliminate the blushing is to apply stop-off
paint on the metal member. It should be
also mentioned that machine marks on
the metal surface promote blushing.
As described earlier, high thermal stress
can be created at the joint because of the
thermal expansion mismatch between the
ceramic and metal members. One of the
methods to reduce the thermal stress is
to closely match the thermal expansion
coefficients of the metal and the ceramic.
For example, molybdenum can be used
to bond with an alumina ceramic (see Ta-
ble II). However, there are a limited num-
ber of the ceramic-metal combinations to
'Spang Industries, Magnetics Division, Butlep, PA.
Fig. 1. Blushing behaviors of the Cusil-ABA@on different substrates. No blushing is observed
on (A) alumina, (B) 304 stainless steel, or (C) copper, whereas extensive blushing is observed
on (0) nickel.
Table II. Thermal Expansion Coefficients of Structural
Ceramics and Common Metals
Material
Silicon nitride
Alumina (99.5%)
Molybdenum
Kovar@
Alloy 42
410 stainless steel
Copper
Thermal expansioncoefficient
(xlO-6C-I)
3.2
8.0
5.7
10.0
10.2
14.0
20.0
satisfy this condition. In the present in-
vestigation, alloy 42t (Fe-4lNi), which
also has a similar thermal expansion coef-
ficient to that of the alumina ceramic, is
used as the metal member.
Another method to reduce the thermal
stress is to use a metal having a low yield
strength. Plastic deformation of the metal
member accommodates the thermal ex-
pansion mismatch, thereby reducing the
thermal stress at the joint. In the present
investigation, two alloy 42 materials with
different strength levels are examined. One
material is in the cold-worked % hard (%
H) condition and has a hardness of 75 in
Rockwell Bscale (Rb). The other material
has been fully annealed at 975C for I
h. The hardness of the annealed material
is 65 in Rockwell B scale.
Filler-MetalComponent
The basic and most important require-
ment for the active filler metal is that the
filler metal should be able to wet and bond
strongly with the ceramic. However, there
are additional requirements on the active
filler metal. As described previously, the
filler metal should not blush over the ce-
ramic or the metal member. Figure 2
demonstrates the effect of the filler metal
on blushing behavior. Two different filler
metals, a 70Ti-15Cu-15Ni alloy and the
Cusil-ABA@,are melted on the alumina
substrate. The 70Ti-15Cu-15Ni alloy
shows extensive blushing because of the
high titanium concentration. In contrast,
the Cusil-ABA@ (2 wt% Ti) shows no
blushing. It is also important that the fill-
er metal is ductile. The ductile filler metal
accommodates the thermal expansion
mismatch to reduce the thermal stress at
the joint as in the case of the ductile metal
member described previously. Also, the
filler metal should have low vapor pres-
sure. In addition, the filler metal should
have the ability to be tailored for specific
applications that require specific proper-
ties such as melting temperature, oxida-
tion and/or corrosion resistance, density,
thermal expansion, etc.
As described earlier, the copper-silver
alloy containing 2 wt% titanium is used
as the filler metal in the present investi-
gation. The thickness of the filler metal
has been chosen as one of the process var-
iables. Foils with three different thick-
nesses (50, 100, and 150 tLm) have been
prepared and the effects of the filler-metal
thickness on the joint properties are eval-
uated.
Engineering Joint Design
As previously stated, one of the major
problems of joining ceramic to metal is
f'TN> Al\KIf' UTn T I<',[,T1\1 \TnT. I':R Nn Q 1 QRQ Ira Arpr~) '~nn
the thermal expansion mismatch between
the ceramic and the metal. The difference
of the thermal expansion coefficients leads
to the high thermal stress in the joint re-
gion. The thermal stress can be reduced
1;>ythe selection of the materials, as dis-
cussed in the Joining Materials section.
As the size of the joint assembly increas-
es, however, the thermal stress also in-
creases, and it becomes more difficult to
overcome the thermal stress by the ma-
terials selections. Oftentimes, this diffi-
culty can be overcome by engineering joint
designs.
CompliantJomtDes~n
Edge brazing of a metal cylinder to a
ceramic face is a popular form of com-
pliant joint. In this case, the thermal ex-
pansion mismatch is accommodated by
the concentric distortion of the metal cyl-
inder. In addition, the fillet formed at the
joint distributes the thermal stress over a
large surface area of the ceramic, and,
hence, the thermal stress on the ceramic
is reduced. Figure 3 shows an example of
such a design, where a copper-clad 430-
stainless-steel cup has been brazed on an
end of an alumina tube. Honeycomb
structures or Feltmetal@~can also be used
to have compliant joints, where distor-
tions in the honeycomb structure or in the
Feitmetal@reduce the thermal stress. One
of the disadvantages of these two designs
is that the joints cannot sustain compres-
sive loading.
Ductile metal interlayer(s) can be used
in the joint assembly. The ductile inter-
layer deforms plastically to reduce the
thermal stress. Another method to obtain
compliant joints is to use an interlayer(s)
that has a thermal expansion coefficient
between those of the ceramic and the
metal. This distributes the thermal ex-
pansion mismatch and reduces the ther-
mal stress. Figure 4 shows an example of
such a joint, known as a gradient seal. In
this case, a molybdenum interlayer (ther-
mal expansion coefficient of 5.7 x 10-6
C-I) is utilized to braze a silicon nitride
(thermal expansion coefficient of 3.2 x
10-6 C-I) disk to a ductile cast-iron
(thermal expansioncoefficientof 12 x 10-6
C-I) substrate.
Compression Joint Design
In this joint, the thermal expansion
mismatch is utilized as an advantage to
obtain the reliable joint. This is achieved
by brazing the ceramic member into the
metal member. During cooling from the
brazing temperature to room tempera-
ture, the metal member (outside) con-
tracts more than the ceramic member (in-
side). This results in compressive stress in
the ceramic member as well as in the joint,
and the joint strength is increased. An
example of such a joint is shown in Fig.
IEnergy Conservation Systems, Brunswick Technit-
ics Division, DeLand, FL.
Fig. 2. Effects of titaniumconcentration on blushing behaviors of active brazing metals on
alumina: (left)extensive blushing is shown for 70Ti-15Cu-15Ni melted at 1050C and (right)
no blushing is observed for the Cusil-ABA@melted at 830C.
M
Copper -clad
stainless steel
~ ~
Cusil-ABA
filler metal
Alumina
cylinder
.,";Jt' :*'~~~E: ::1 -.-.-
Fig. 3. Example of the edge brazing where a copper-clad 430-stainless-steel cap has been
brazed on an alumina cylinder: (left)a schematic cross section of the assembly and (right)
the actual brazed sample.
~
-~, ,~, ,,~,~, VM V" ,~,.,."" .~"'".,."
Si 3N4 Ceramic
Cusil-ABA
. !!!J Molybdenum
Cusil-ABA
m
""""" ""'""<..",,,, ~""~" """'~"""""""""
-
Dulile cast iron
Fig.4. Exampleof the gradient seal where a siliconnitridedisk has been brazed on a ductile
cast-iron plate with a molybdenuminterlayer: (left)a schematic cross section of the seal and
(right) the actual brazed seal.
1593 CERAMIC BULLETIN, VOL. 68, NO.9, 1989 (@ACerS)
.L-
5, where a silicon nitride rod is brazed to
410 stainless steel through the compres-
sion joint. It should be noticed that the
silicon nitride rod has a tapered end.
Therefore, the stainless steel has a hole
with the same taper and the end of the
steel has a knife edge. This is to eliminate
sudden changes in the stress that can be
detrimental for the joint properties.
Stress-Distribution Joint Design
A ceramic backup can be used to dis-
tribute tensile loading on the metal dia-
phragm. Figure 6 shows an example of
this type joint, where a cupronickel sheet
has been brazed on an alumina cylinder.
As shown in Fig. 6, a backup ring of alu-
mina has also been brazed on top of the
cupronickel sheet. The backup ring serves
two purposes. First, the backup ring cre-
ates additional interface area (at the cu-
pronickel sheet and the backup ring); thus,
the thermal stress is distributed at two
interfaces instead of one. Second, the
backup ring changes the stress distribu-
tion in the cupronickel sheet so that there
is no peeling moment at the edge of the
cupronickel sheet.
Brazing Procedures
Furnace brazing is the best technique
for ceramic-metal joining by the active
filler metal. Vacuum or inert gas is the
most economical and pollution-free op-
eration. In the case of vacuum brazing, a
leak rate should be controlled to be less
than 0.005 mm Hg/h. In the case of inert-
gas brazing, a dry Ar, He, or H2 atmo-
sphere can be used. Ironically, one of the
major problems related to active filler
metal brazing is that the active element
wets nearly all materials. Therefore, care
should be taken in designing the joint as-
sembly so that molten filler metal does
not touch any part of the brazing fixture.
The heating rate 'during the brazing is
important. Since the metal member has
higher thermal conductivity than the ce-
ramic member, the metal can heat up faster
than the ceramic. In this event, the filler
metal is drawn away by the metal mem-
ber. This becomes more important in the
applications where the mass of the metal
member is much smaller than that of the
ceramic (e.g., the edge brazing). There-
fore, the heating rate should be controlled
carefully to minimize the temperature dif-
ference betweenthe ceramic and the metal.
This can be achieved by initially holding
the temperature just belowthe solidus and
then increasing the temperature at a con-
trolled rate to the brazing temperature.
The cooling rate is also critical for the
reliable joints. When the cooling rate is
too fast, there is insufficient time for the
filler metal and/or the metal member to
deform plastically and reduce the thermal
stress. Therefore, the cooling rate should
Westinghouse Electric Corp., Pittsburgh, PA.
be controlled to minimize the residual
stress. In both the heating and cooling
processes, the slower the rate of temper-
ature change, the better the resultant joint
properties. However, the temperature
changes should be fast enough to mini-
mize the processing cost.
Considering all the factors mentioned,
preliminary experiments have been con-
ducted to optimize brazing procedures for
the present investigation. The results lead
to the temperature-time profile shown in
Fig. 7. This profile is utilized throughout
the present investigation unless otherwise
mentioned.
Testing Methods
There are three major requirements for
a testing method to evaluate the mechan-
ical properties of the ceramic-metaljoints.
First, a testing method should lead to ac-
curate and consistent results. Second, a
testing method should be able to evaluate
effects of processing variables on the joint
properties. Third, the results of the tests
should provide meaningful engineering
parameters that can be utilized for de-
signing the ceramic-metal joints. There
are many testing methods used for eval-
uating the joint properties. Three fre-
quently used methods will be reviewed.
In addition, a new testing method will be
introduced and examined.
01
&I
Copper Tube
II
Si 3N4 C"ami,
410SlaJo'",S'oo'
j
Fig. 6. Example of the stress-distribution
joint. Alloy42 sheets are brazed on both
ends of an alumina cylinder with alumina
backup rings: (top) a schematic cross sec-
tionof thejoint and (bottom)the actual stress-
distributionjoint.
ined. The detailed descriptions for the peel
test have been given in Ref. 7. The results
are shown in Fig. 9. A group of six results
shown on the left side of Fig. 9 is obtained
on the ground-and-resintered surface. High
peel strengths (=20 lb (90 N)) have been
obtained in all six tests. The results shown
on the right side of Fig. 9 have been ob-
tained on the ground surface. Again, con-
sistent results are obtained. Peel strengths
of the ground surface (=6 lb (27 N)) are
~~~'Hm ~TnT~mnT Hr.T ~O "Tr. '"' ""'0'"' {r?\Af"~_"\
"",ii-ABA fill" m,1aJ
1-- --
. ~~-~
Fig. 5. Example of the compression joint.
A silicon nitride rod is brazed into a hole ma-
chined in a 410 stainless steel with Incusil-
ABA@* (top) a schematic cross section of
the joint and (bottom) the actual compres-
sion joint.
Peel Test
In the peel test, a metal strip is brazed
on a ceramic substrate by the active filler
metal. The load required to peel the metal
strip from the ceramic substrate is mea-
sured. Therefore, the peel test is relatively
simple and cheap. Examples of the peel
test are shown in Fig. 8, where three Ko-
var@strips have been brazed to alumina
substrate by Cusil-ABA@(50-I.LIDthick).
Two different surface conditions of the
alumina (AL-995) substrate are exam-
.
-
Alloy 42
IIIII!IIIII
- IIIIIIIIIIIIII Cusil-ABA
I
AluminaCylinder
- IIIIIIIIIIIIIICusil-ABA
Alloy 42
!IIIIIIIIIIiII III!IIII!iIiII Cusil-ABA
II II
Alumina backup ring
considerably lower than those of the
ground-and-resintered surface. This is due
to surface damages on the ground ceram-
ic as described earlier. Figure lO shows
cross-sectional views of the untested peel
test samples. The interface between the
Kovar@and the ground-and-resintered ce-
ramic is very smooth (Fig. lO(A and
resulted in the high peel strength. The
interface between the Kovar@ and the
ground ceramic is not smooth and also
contains small cracks (Fig. 10(B. As a
result, low peel strength has been ob-
tained.
These results demonstrate that the peel
test is a useful method for evaluating joint
properties. It is simple and cheap, and the
results are consistent. Also, effects of the
processing parameters can be detected.
However, one of the disadvantages of the
peel test is that the result of the peel test
cannot be translated into meaningful en-
gineering parameters for designing of ce-
ramic-metal joints.
Tensile Test
The ASTM F19-61 CLM-15 tensile
test]2 is examined for the evaluation of
the ceramic-metal joint by the active
brazing metal. Figure II shows the test
sample assembly, brazed sample, and
fractured sample. As shown in Fig. II, a
Kovar@ring is brazed to two alumina ce-
ramic parts with Cusil-ABA@.Again, two
surface conditions of the ceramic are
tested: ground and ground-and-resintered
surfaces. The results demonstrate that the
tensile test can also detect the effect of
the ceramic surface conditions. The frac-
ture strength of the sample with the
ground-and-resintered ceramic is 75 MPa
(10.8 ksi), whereas that of the sample with
the ground ceramic is 49 MPa (7.1 ksi).
In the majority of the tensile tests, how-
ever, failures have occurred predomi-
nantly in the ceramic member instead of
the joint. This is primarily because the
loading mechanism places the ceramic in
tension. When the joint strength is higher
than the tensile fracture strength of the
ceramic, the tensile test becomes ineffec-
tive for evaluating the joint strength.
25
- 20
g
-<=
g> 15
~
1;)
gj 10
Q.
5
Ground and resintered Ground
Fig. 9. Results of the peel tests performed
on the Cusil-ABA@filler metal. High peel
strengths (20 Ib (90 N)) are obtained on the
ground-and-resintered alumina. In contrast,
the peel strengths for the ground substrate
are low (6 Ib (27 N)).
2000
20 min brazing
-Jf-
Liquidus (815'C)
Solidus (780'C)
1500
1000 E
500
2 4 6 8
Time (h)
Fig. 7. Temperature cycle for Cusil-ABA@ brazing.
Fig. 8. Sample assembly and brazed samples for the peel test. Alumina substrate, a foil of
an active filler metal (Cusil-ABA@),and three strips of Kovar@are shown at the bottom of
the figure. At the top-right of the figure is a brazed sample and at the top-left is the sample
where one Kovar@strip has been peeled off from the substrate.
Shear Test
The shear test provides important in-
formation on the mechanical properties of
the joint, namely shear strength. Figure
12 schematically illustrates two common-
ly used shear tests. In the test shown on
the left side of Fig. 12, two blocks of the
materials are brazed together and pushed
in opposite directions.]) The major prob-
lem in this type of shear test is that a
rotating moment can act on the specimen
because of the loading mechanism.
Therefore, to eliminate the rotation of the
sample, a hold-down force (FH) is re-
quired. The hold-down force leads to a
compressive stress at the joint, and, hence,
the shear stress measured will depend on
the hold-down force. The larger FH, the
larger the shear strength. The fillet at the
joint can also affect the result when the
size of the test blocks are not sufficiently
large, compared with the fillet size.
Therefore, the accurate evaluation of the
joint shear strength cannot be performed
in this type of shear test. Another com-
mon type of the shear test is shown on
the right side of Fig. 12. In this case, a
ceramic rod is brazed in a metal ring. The
ceramic rod is then pushed and the shear
strength of the joint is determined. How-
CERAMIC BULLETIN, VOL. 68, NO.9, 1989 (@ACerS) 1595
1200
1000
800
S5
ill
:; 600
a;
Q;
0..
E
400
200
0
]
0
--
.. - ...
-
16Gsil~ABB I
,-" . I
Fig. 10. Scanning electron micrographs taken at the brazed joints, (A) The interface between the filler metal (Cusil-ABA@)and the ground-
and-resintered alumina is very smooth, whereas (B) that between the filler metal and the ground alumina contains small cracks,
ever, because of the thermal expansion
mismatch between the ceramic rod and
metal ring, the joint is in compressivestress
(as in the case of the compression joint
as described previously). The compres-
sive stress depends on process variables,
e.g., a gap between the ceramic rod and
the metal ring, cooling rate, etc. There-
fore, changes in the process variables af-
fect both the shear strength of the joint
and the compressive stress at the joint.
As a result, the effects of the process var-
iables on the shear strength cannot be
properly evaluated in this type of test.
Double-Brazed Shear Test
A new type of the shear test, namely a
double-brazed shear (DBS) test, is uti-
lized in the present investigation, The ba-
sic principle of the DBS test is illustrated
schematicallyinFig. 13.Threeblocksare
Material B
F2
FI-'
Fig, 13. Schematic illustration of the dou-
ble-brazed shear test.
Fig, 11, (L-R) Test-specimenassemblies (ceramic-filler metal-metal-filler metal-ceramic and
ceramic-filler metal-ceramic), a brazed sample, and a tested sample for tensile test. The
assembly shown on the left includes metal-ceramic joints and, hence, is used for the present
investigation,
Fs
FH
Fs
Braze
FH
Ceramic Block on Metal Block
Fs
Ceramic rod
Braze
Fs Fs
Ceramic Rod in Metal Ring
F2
Fig, 12, Schematic illustrations of two common types of shear tests on brazed joints,
1596 CERAMIC BULLETIN, VOL. 68, NO.9, 1989 (@ACerS)
- --- -
~
~
-
."
Fig. 14. (L-R) Test-specimen assembly, a brazed sample, and a
tested sample for the double-brazed shear test.
.
I
Fig. 15. Test apparatus for the double-brazed shear test.
butt-brazedtogetherandthecenterblock
is pushed against the two end blocks.
Therefore, shearstressis applied on two
brazedjoints simultaneously.That is, the
propertiesof two joints can be tested in
a singleDBS test. It is found, however,
that theshearstrengthsof bothjointscan-
not be determinedby a singletest. This
is because once onejoint (the weaker one)
fractures, the loading condition on the
other joint becomes undesirable (this point
will be explained in detail later). Conse-
quently, one DBS test provides the fol-
lowinginformation:0) it provides the shear
strength of the weaker joint and (ii) it can
determine which joint is weaker. There-
fore, when two different materials are used
at the end blocks, one can measure the
shear strength of the weaker joint and also
determine which material forms the
stronger joint with the material used as
the center block. When the same material
is used as the end blocks, the shear strength
of the weakerjoint obtainedby the DBS
test provides a safety factor for the design
engineer.
Figure 14 shows the test specimen as-
sembly, before and after brazing and also
after testing. The material for the center
block is alumina ceramic (AL-995) and
the two end blocks are alloy 42 (Fe-41Ni).
All three blocks have the same dimen-
sions of 12.4 mm X 12.4 mm x 15.9 mm
(0.490 in. X0.490 in. x 0.625 in.). Cusil-
ABA@is used as a filler metal. Brazing
is performed at 830C for 20 min. After
the brazing, two opposite surfaces of the
brazed specimen are ground to assure that
these two surfaces are parallel to each
other for proper loading.
The DBS test apparatus is shown in
Fig. 15. The brazed sample, also shown
in Fig. 15, has been coated by amorphous
boron nitride powder to prevent friction.
It is then inserted in the test apparatus
through square holes on two facing side-
walls. Therefore, no hold-down load is
~Instron Corp., Canton, MA.
Processing Conditions for Double-Brazed Shear Test Specimens
Filler metal
thickness Cooling rate
Ceramic Metal (I'm (in.)) (OC/min)
Table II!.
SP'Ccimen
A Ground and resintered*
B Ground
C Ground and resintered
D Ground and resintered
E Ground and resintered
F Ground and resintered
*1650Cfor I h. '975C for I h.
necessary. End covers attached to the walls
prevent fractured fragments from flying
out through the holes. These covers do
not touch the specimen, and, hence, no
additional stresses can be applied on the
specimen. After aligning the specimen
carefully, a plunger is inserted into the
main cavity of the assembly. The bottom
of the plunger is flat so that the load is
applied over a whole area of the center
block. The test assembly with the speci-
men is placed in an Instron testing ma-
chine.~The plunger is pushed under a
constantcrossheadspeedof 0.25mm/min
(0.01 in./min), and the load is recorded
by a strip chart recorder.
ProcessVariableEffects
Effects of four major process variables
on the joint properties are examined by
the DBS test. They are surface condition
of the ceramic member, strength level of
the metal member, thickness of the filler
metal, and cooling rate during brazing.
Processing conditions are summarized in
Table III. For specimen A, the ground-
and-resintered ceramic material and an-
nealedalloy42 havebeenbrazed by a 50-
~m-thick foil of the Cusil-ABA@. The
cooling rate is 5C/min, which is a stan-
dard cooling rate as shown in Fig. 7. This
condition has been regarded as a base
condition.For each of the remainingfive
specimens, only one of the four variables
is changed and the other three variables
are kept constant so that effects of a sin-
gle variable can be determined. For spec-
imen B, the surface of the ceramic ma-
Annealed'
Annealed
As-received (3/4 H)
Annealed
Annealed
Annealed
50 (0.002)
50 (0.002)
50 (0.002)
100 (0.004)
150 (0.006)
50 (0.002)
5
5
5
5
5
1
terial is in as-ground condition. In this
case, two shear stress orientations, normal
and parallel to the grinding direction, are
utilized to investigate effects of shear stress
orientation relative to the grinding direc-
tion on the shear strength. For specimen
C, an as-received alloy 42 is used. The
as-received alloy 42 is in 3/4 H condition
and has a hardness of 75 on the Rockwell
B scale. In contrast, the annealed alloy
42 has a lower hardness of 65 on the
Rockwell B scale. Specimens D and E are
brazed by thick foils of the Cusil-ABA@,
100 ~m and 150 ~m, respectively. A slow
cooling rate (1C/min) is used for braz-
ing of specimen F.
In all of the tests, one joint fractures
before the other, as expected. Figure 16
shows a typical load-displacement curve
of the DBS test. (Displacementin Fig. 16
indicates the crosshead displacement and,
hence, includes displacements of the test
O.OOI-in. displacement
'---'
4000
-;;; 3000
g
"0
'"
.3 2000
1000
Fig. 16. Typical load-displacement curve
obtained by the double-brazed shear test
(specimen D).
1597
CERAMIC BULLETIN, VOL. 68, NO.9, 1989 (@ACerS)
IAIoy 42U
t
l
Cusil-ABA .'
,"
".
l
I
Cusil-ABA
IAlloy42r.......
L
I
I
- -- - - - -_J
apparatus and testing machine as well as
the test specimen.) One joint has frac-
tured at 1750 Ib (7785 N), and then the
other joint has fractured at 3500 Ib (15570
N). The load for the second fracture is
much higher than that for the first frac-
ture, because when one brazed joint frac-
tures, the specimen isjammed in the main
cavity. In most DBS tests, therefore, test-
ing is terminated after the first fracture.
The shear strength is calculated simply
by dividing the load at the first fracture
over a total area of two brazed surfaces.
The results of the DBS tests are sum-
marized in Table IV. In general, the stan-
dard deviations are relatively small, in-
dicating that the DBS test has produced
consistent results. However, specimen E
shows a large standard deviation. Speci-
men E has a thick filler metal (150 /lm).
It is observed that molten filler metal has
seeped out from the joining surfaces dur-
ing brazing. Therefore, the thickness of
the filler metal after the brazing is not
uniform and varies from one specimen to
another. As a result, the standard devia-
tion for specimen E becomes large. It is
also demonstrated in Table IV that the
DBS test is sensitive to the process var-
iables.
(A) ,
r'
~
I
relative to the grinding direction are also
investigated. When the shear loading is
applied normal to the grinding direction,
all specimens except one break at very
low loads so that the shear strengths can
not be determined accurately. These re-
sults indicate that the shear strength nor-
mal to the grinding direction is lower than
that parallel to the grinding direction. It
should be mentioned that the shear
strength and standard deviation values in
Table IV are calculated from the results
of all of the DBS tests performed on spec-
imen B.
StrengthLevelof theMetal
The results for specimen C demon-
strate that the strength level of the metal
joint properties. When the filler metal
thickness is increased to 100 /lm (speci-
men D) from 50 /lm (specimen A), an
increase in the shear stress' is observed.
There are two possible explanations for
these results. First, the thicker filler metal
contains more titanium atoms available
to bond with the ceramic. Second, the
thicker filler metal provides more plastic
deformation during the cooling cycle to
result in lower thermal stress at the joint.
When the thickness of the filler metal is
increased to 150 /lm, however, the results
of the DBS tests become more scattered.
As described earlier, this is due to the fact
that the filler metal has seeped out from
the joining surface.
Table IV. Results of the Double-Brazed Shear Tests
Standard
deviation
MPa psi
2.0
1.5
3.6
1.0
7.4
0.8
300
220
530
140
1075
111
~
.
..-
JI"\
:}
I
~'
.
'
.'
rl
I
~ -=- J
lqusil~BA1
- ..,.
--,
')
~Usn:-AB~I
- ~ "I
Fig. 17. Scanning electron micrographs of the joint interfaces between the filler metal and ceramic member. (A) The interface between the
filler metal and the ground-and-resintered alumina is very smooth, whereas (B) that between the filler metal and the ground alumina contains
cracks at the interface.
Surface Condition of the Ceramic
Specimen B, with the ground ceramic,
has the lowest shear strength (6.2 MPa).
This indicates that the surface condition
of the ceramic member is very critical for
the reliable joint. This result agrees with
those obtained in the peel test and tensile
test. The damaged surface layer on the
ground ceramic leads to the low shear
strength. Figure 17 shows the cross-sec-
tional views of the joints for specimens A
and B at a high magnification. Specimen
A shows a defect-free interface (Fig.
17(A, whereas specimen B contains
cracks parallel to the interface (Fig. 17(8)).
The effects of the shear stress orientation
member is also important. When the un-
annealedalloy 42 (Rb=75) is used, the
shear strength of the joint is 9.4 MPa,
compared with that obtained in specimen
A (20.5 MPa) with the annealed alloy 42
(Rb=65). The metal member can deform
plastically to reduce the thermal stress.
The amount of the plastic deformation
dependsonthe strengthlevelof the metal
member.The lowerthe strength, the more
the amount of plastic deformation. As a
result, the metal member with the lower
strength level leads to the lower thermal
stress at the joint which, in turn, increases
the joint strength.
Filler-MetalThickness
The filler-metalthicknessinfluencesthe
30
20
co
a.
6
10
a
B C
Specimen
0
Fig. 18. Summary of the OBS tests for
specimens A through O. Bars indicate the
average shear strength and solid circles in-
dicate data points. It is demonstrated that
the OBS test is sensitive to process varia-
bles.
1598 CERAMIC BULLETIN, VOL. 68, NO.9, 1989 (@ACerS)
Averageshear
Number strength
Specimen
of tests MPa
psi
A 4 20.5 2980
B 4 6.2 900
C 3 9.4 1360
D 2 26.5 3840
E 3 19.6 2845
F 2 18.9 2740
5000
'iji 4000
E,
-<:
0, 3000
c
Q)
1;5 2000
m
Q)
-<:
(j) 1000
0
A
Alloy 42
.-
----.
Cooling Rate During Brazing
Finally, the effects of the cooling rate
during brazing are investigated. Two
coolingrates, 5Cjmin and I Cjmin, are
utilized. As demonstrated in Table IV
(specimens A and F), there is no detect-
able difference in the shear strengths be-
tween the two cooling rates.
Experimental Results
Figure 18 shows the results of the DBS
tests for specimens A through D in a
graphical manner. Bars indicate the av-
erage shear strengths and solid circles in-
dicate data points. As described previ-
ously, the effects of the process variables
on the shear strength are clearly shown.
It should be also mentioned that all of the
data points for each specimen show small
scatters, which indicate consistency in the
DBS test.
Figure 19 shows four broken samples
(one for each of specimens A through D).
In all tests, cracks have initiated at the
right side of the samples. This might sug-
gest that a small bending moment has been
applied on the sample and has produced
a tensile stress at the right-side surface.
Although cracks have initiated at the same
place, the crack-propagation path varies
depending on the specimen. For speci-
mens A and D which show high shear
strengths (see Table IV), the crack ini-
tially has propagated at the joint interface
and then has changed direction by ap-
proximately 45 into the ceramic. For
specimen B, the crack simply propagated
at the joint interface. This is due to the
fact that the joint strength is very low (6.2
MPa). Specimen C shows that the crack
propagated along the joint, but in the ce-
ramic. The high-strength metal in speci-
Fig. 19. Brokentest samples for specimens Athrough D. Inallcases, the cracks are initiated
at the right side of the sample. However, the crack-propagation paths are shown to be
dependent on the conditions of the specimen preparations.
men C does not deform plastically to re-
duce the thermal stress during the cooling
cycle. As a result, the ceramic in the vi-
cinity of the joint might have been dam-
aged and provided the path for the crack
propagation.
These results indicate that the DBS test
can be the optimum testing method for
the evaluation of the joint strength be-
tween the ceramic and the metal. The DBS
test provides consistent results and also is
sensitive to the process variables. Fur-
thermore, the shear strength values which
are obtained by the DBS tests can be used
directly for the engineering design of ce-
ramic-metal joints. However, the results
of the DBS tests also demonstrate that all
process variables should be well-defined
when designing high-reliability joints be-
tween ceramics and metals.
Conclusions
(I) High-reliabilityjoiningof ceramic
to metal requires complete understanding
of each and every process variable.
(2) The double-brazed shear test pro-
vides a meaningful engineering parame-
ter for design purposes.
(3) The double-brazed shear test is
sensitive to process variables in the braz-
ing operation.
(4) Ceramic surface preparation is the
most critical parameter to obtain a reli-
able ceramic-metal joint.
(5) Use of a metal with a lower yield
strength results in higher shear strength
at the brazed joint.
(6) Thicker filler metal generally leads
to higher shear strength.
(7) The results of the double-brazed
shear tests demonstrate that all process
variables should be clearly defined to op-
timize engineering design (e.g., finite-ele-
ment method) of joints between ceramics
and metals.
Acknowledgments
The authors are deeply indebted to Mr. J."Rosek
and Mr. R. Spano, both members of WESGO R&D,
for their technical support and helpful discussions.
References
'H. Pulfrich, "Ceramic to Metal Seals," U.S. Pat.
Nos. 2163407 and 2 163410, June, 1939.
'H. J. Nolte and R. F. Spurch, "Metallizing and
Ceramic Sealing with Manganese," U.S. Pat. Nos.
2667432 and 2667427, Jan. 24, 1954.
JA. J. Chick and L. J. Speck, "Fabrication of Metal-
to-Ceramic Seals," U.S. Pat. No.2 708 787, May,
1955.
'C. S. Pearsall, "New Brazing Methods for Joining
Non-Metallic Material to Metals," Mater. Methods,
30, 61-62 (1942).
'F. C. Kelly, "Metallizing and Bonding Non-Me-
tallic Bodies," U.S. Pat. No.2 570 248, Oct. 9, 1955.
'H. Mizuhara, "Process of Making a Composite
Brazing Alloy of Titanium, Copper and Nickel," U.S.
Pat. No.3 561 099, Feb. 9, 1971.
'H. Mizuhara and K. Mally, "Ceramic-to-Metal
Joining with Active Brazing Metal," Weld. J., 64 [10]
27-32 (1985).
'E. Lugscheider, H. Krappits, and H. Mizuhara,
"Joining of Non-Metallized Ceramic with Metals by
Insert of Ductile Active Brazing"; presented at the
Second International Colloquium, Joining of Ceram-
ic, Glass, and Metal. Bad Nauheim, FRG, 1985.
"A. J. Moorhead and H. Keating, "Direct Brazing
of Ceramics for Advanced Heavy-Duty Diesels," Weld.
J.,65 [10] 17-31 (1986).
"'H. Mizuhara and E. Huebel, "Joining Ceramic
to Metal with Ductile Filler Metal," Weld. J., 65 [10]
43-51 (1986).
"H. Mizuhara, "Vacuum Brazing Ceramics to
Metals,"Adv. Mater. Processes,13 [2]53-55(1987).
""Tension and Vacuum Testing Metalized Ceramic
Seals," ASTM Specification F19-64. 1964 Annual
Book of ASTM Standards, Part 8. American Society
for Testing and Materials, Philadelphia, PA.
1Jw.H. Sutton, "Wetting and Adherence of Ni/Ni
Alloys to Sapphire," GE Space Sciences Laboratory,
Rept.R-64SD44, Philadelphia, PA,1964. .
CERAMIC BULLETIN, VOL. 68, NO.9, 1989 (@ACerS) 1599