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International Journal of Adhesion & Adhesives 29 (2009) 234– 239

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International Journal of Adhesion & Adhesives

journal homepage: www.elsevier.com/locate/ijadhadh

Adhesive defect density estimation applying the acoustic emission technique

D. Croccolo , R. Cuppini
DIEM, University of Bologna, Viale Risorgimento, 2, 40136 Bologna, Italy

a r t i c l e in f o a b s t r a c t

Article history: The aim of this work is to study in depth the use of the acoustic emissions, as a non-destructive testing
Accepted 18 March 2008 technique, applied to the adhesively bonded joints. In a previous paper, three defect densities of the
Available online 10 June 2008 adhesive, 0%, 50% and 100%, were investigated, while in the present work two more intermediate values
Keywords: have been considered: 25% and 75%. The first goal of this paper is to confirm the good correlation,
Anaerobic highlighted in the previous one, between the adhesive defect density and the cumulative counts of the
Metals acoustic emissions; the second goal is to improve a methodology which might be capable of estimating,
Non-destructive testing with accuracy, the adhesive bonding defect and the final releasing moment of the assembled joints. In
Shaft–hub couplings this paper, the new results have been integrated with the previous ones and a more detailed map of the
adhesive slope variations is presented.
& 2008 Elsevier Ltd. All rights reserved.

1. Introduction of the structure during a single loading test. Hence, the AE

The acoustic emissions (AE) uttered by the stressed materials
are the stress waves produced by sudden movement of a crack.
Hence, the source of AE is a defect-related process caused by a
crack propagation or by a rapid plastic deformation. The rapid
deformation, in fact, produces a stress wave which radiates into
the structure and may excite a sensitive piezoelectric transducer.
As the stress and the crack propagation or the plastic rapid
deformation rise in the material, the emissions generated rise too.
The signals acquired by the sensors are, usually, amplified and
plotted in order to define the tensile state of the material.
Therefore, AE inspection is usually carried out during a controlled
loading test of the structure.
AE differ from the other non-destructive testing (NDT)
methods mainly because the signal is produced by the material
itself, not by an external source, and because the AE detect the
micro-movements, while the other methods detect the geome-
trical discontinuities; the other differences are summarized in
Table 1. It is widely demonstrated in the literature that the most
common NDT techniques (for instance, radiography, ultrasounds,
parasitic currents and magnetic particle) are not able to estimate
the density of the adhesive bonding defects produced by a lack of
glue, unclean surfaces, and an insufficient degree of polymeriza-
tion once the parts are assembled together [1,2]. On the contrary,
one of the benefits of the AE inspection is that it is possible to
perform a non-intrusive inspection applied to the whole volume
 Corresponding author. Tel./fax: +39 0512093413.
E-mail addresses: dario.croccolo@unibo.it (D. Croccolo),
rossano.cuppini@mail.ing.unibo.it (R. Cuppini).
technique can be successfully applied in order to evaluate the
density of the adhesive defects as a NDT method if the value of the
maximum load applied during the tests is sufficiently lower than
the failure load of the joint [3–5].
AE inspection is a powerful aid for the study of the failure of
adhesively bonded joints because it is strictly related to the
adhesive strength, and to its damage. Some recent works pointed
out a strong correlation between the failure load of the joints and
the cumulative counts of the emissions, and between the defect
density of the adhesive and the cumulative counts of the
emissions [6–12].
Therefore, encouraged by the good results obtained in [12], we
decided to study in depth the correlation between the adhesive
bonding defects and the AE adding some other intermediate levels
of defect density. In the present work, we analyzed and added the
correlations of 25% and 75% defect density in order to define the
complete map of the cumulative counts slope variations and to
forecast, more accurately, the releasing moment of the joints.
2. Methodology
The test specimen, shown in the drawing of Fig. 1 and in the
pictures of Figs. 2 and 3, was designed and manufactured by the
authors with the aim and the scope presented in [12]. After each
test the specimen was disengaged, cleaned using the Loctite 7063
cleaner and a cutter, and reused for a new test. The female part of
the specimen, Fig. 2, and the male one, Fig. 3, are in 18NiCrMo3
face-hardened steel and are held together with a screw and a nut.

0143-7496/$ - see front matter & 2008 Elsevier Ltd. All rights reserved.
doi:10.1016/j.ijadhadh.2008.06.001
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D. Croccolo, R. Cuppini / International Journal of Adhesion & Adhesives 29 (2009) 234–239 235

The fundamental dimensions of the specimen, as reported in the When the adhesive defect was simulated on the specimen,
drawing of Fig. 1, are summarized in the following list: there was another step (spreading the contact surfaces with a film
of lube oil) between #2 and #3.
 mean coupling diameter Dm ¼ 99.13 mm;
 coupling axial length L ¼ 25 mm;
2.2. Tests run
 taper angle a ¼ 21;
 external diameter of the female part DAa ¼ 141.6 mm;
 QA ¼ Dm/DAa ¼ 0.7. The new additional tests were performed with two defect
densities (25% and 75%) and the same three interference levels,
already used for the previous tests with adhesive defect density
2.1. Specimen setting-up cycle
equal to 0%, 50% and 100%. The new tests were performed with the
aim to complete the previous design of experiment (DOE) data set
The specimen setting-up cycle is realized by the following
and to obtain a more detailed response surface for the failure load
steps:
(releasing moment) of the adhesive (Mad), which has been
calculated in each test by subtracting the moment due to the
1. disengaging the specimen;
interference (Mint) from the total releasing moment (Mtot)
2. cleaning the contact surfaces using the Loctite 7063 cleaner
measured by the torque machine, following the same methodol-
and a cutter;
ogy presented in [12].
3. spreading the contact surfaces with the Loctite 638 adhesive;
The minimum polymerization time was established at 72 h,
4. generating the contact pressure using a hydraulic press (the
which is the inferior limit needed for a good polymerization of the
pressure is measured using a strain gauge applied on the
adhesive. The load speed variation was set at 15 Nm/s in order to
external diameter of the female part of the specimen);
obtain a quasi-static loading test.
5. tightening the nut in order to maintain the axial load;
Hence, the global factorial plane (three interference levels and
6. waiting for the adhesive polymerization in an oven at the
five adhesive defect density levels) has 15 points and the total
constant temperature of 40 1C for 72 h.
number of tests is equal to 60, since we performed 4 replications
for each point. The number of additional tests is 24. The complete
Table 1 ranges of the factors are the following:
Characteristic of acoustic emission inspection compared with other methods

Acoustic emission Other methods  interference:

Detects movement of defects
Requires stress
Each loading is unique
More material sensitive
Less geometry sensitive
Less intrusive on plant/process
Requires access only at sensor
Tests whole structure at once
Main problems: noise related
Detect geometric forms of defects
Do not requires stress
Inspection is directly repeatable
Less material sensitive
More geometry sensitive
More intrusive on plant/process
Requires access to whole area of inspection
Scan local region in sequence
Main problems: geometry related
level 0: 0.002 mm (H7-m6 cylindrical coupling equivalent)
level 1: 0.036 mm (H7-r6 cylindrical coupling equivalent)
level 2: 0.077 mm (H7-t5 cylindrical coupling equivalent)
 adhesive defect presence:
level 0: surfaces completely cleaned
level 0.5: 25% of the surfaces completely oiled
level 1: 50% of the surfaces completely oiled
level 1.5: 75% of the surfaces completely oiled
level 2: 100% of the surfaces completely oiled

L=25mm
Dm =99.13mm
DAa =141.6mm

92°

Fig. 1. Drawing of the specimen.

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236 D. Croccolo, R. Cuppini / International Journal of Adhesion & Adhesives 29 (2009) 234–239
Fig. 2. The female part of the specimen.
Fig. 3. The male part of the specimen.
The defect density (0%, 25%, 50%, 75% and 100%) was simulated
by spreading first a film of lube oil and then the adhesive on the
two contact surfaces of the specimens. The percentage of oiled
surface was equal to the desired defect density (four marks were
put on the female and on the male parts in order to obtain four
sectors exactly equal to a quarter of a circle).
The numerical results of the new analysis, gauged by applying
the DOE and the ANalysis Of VAriance (ANOVA), were presented in
[13], while in the present work they are summarized with the new
response surface shown in Fig. 4. During each test we have also
acquired the AE uttered by the specimens.
3. Results
The AE parameters acquired and analysed with the Physical
Acoustics Corporation1 (PAC) control unit installed on a personal
computer are the cumulative counts and the energy uttered as
acoustic waves. The transducer location, placed on the external
diameter of the female part, is reported in Fig. 5.
1
The specific PAC model employed for the experimental tests was DISP-4,
with a. NANO 30 transducer, 70 dB as sensitivity and 298 kHz as peak frequency.
Fig. 4. The DOE response surface [13].
Fig. 5. The PAC transducer applied on the external surface of the female part.
The correlation coefficients between the releasing moments
and the total cumulative counts and between the releasing
moments and the cumulative counts at 4 kN m have been
calculated. The results analysis confirmed what was discussed
and presented in [12]: the correlation coefficients, computed by
grouping the results with the same adhesive defect density, are
always higher than 0.75, whereas no correlation exists if the
results are grouped with the same interference level. The value of
4 kN m, which is about 30% of the maximum releasing moment of
the coupling (13.16 kN m calculated in [13] with no defect and no
interference), is an appropriate value in order to acquire a
significant number of cumulative counts and to consider the tests
as non-destructive ones.
The diagrams of the cumulative counts related to the applied
load have been cut at the beginning of the slope variations and
were interpolated with the minimum mean square error method
following the same methodology presented in [12]. The slope
variations indicate the transition from the adhesive micro-fracture
zone to the coalescence one [8], which means an imminent
disengaging. For each group of interpolation lines (0%, 25%, 50%,
75% and 100% of the defect density), the average and the standard
deviation values of the slopes have been calculated and the results
are reported in Table 2 and plotted in Fig. 6.
4. Discussion
All the tests, also those with defect density equal to 25% and
75%, confirmed the strong correlation between the failure load
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D. Croccolo, R. Cuppini / International Journal of Adhesion & Adhesives 29 (2009) 234–239 237

and the number of cumulative counts and the good relationship 4 kN m, are always higher than 0.75 for all the five adhesive defect
between the AE slopes and the defect density of the adhesive. As densities.
already observed, the correlation coefficients, between the The five areas between each slope average minus and plus its
maximum applied load and the total cumulative counts and standard deviation, corresponding to each defect density, are
between the maximum applied load and the cumulative counts at plotted in Fig. 6. While the area corresponding to 75% of the defect
density has no superposition zones with the two contiguous areas
(50% and 100%), the one corresponding to 25% of the defect
density is partially superimposed on the 50% area. This occurrence
Table 2
Characteristics of the slopes for each group of interpolation lines (0%, 50% and confirms that the AE correlation decreases when the defect
100% of adhesive defect density) density decreases. Nevertheless, it is possible to consider the
overlapping area between 25% and 50% of the defect density as
Slope (cumulative counts/kN m) Defect density
belonging to (a part of) 50% area. It means that a tested joint with
0% 25% 50% 75% 100% a defect density equal to 25% but with an AE slope included in the
overlapping area would be considered as a 50% defected joint and,
Average (x̄) 221 3801 4969 18,070 63,278 therefore, with a lower Mtot than the actual one. Furthermore, the
Standard deviation (s) 206 2633 2962 9229 34,571 maximum error computed in the evaluation of Mtot is lower than
x̄s 15 1168 1984 8841 28,707
x̄+s 427 6434 7908 27,299 97,849
10% and, anyway, in a safety condition. Hence, the actual
cumulative counts slope map is plotted and presented in Fig. 7.

Fig. 6. Areas between each slope average minus and plus its standard deviation: the sketched area is the overlapping zone between 25% and 50% of adhesive defect density.

Fig. 7. Areas between each slope average minus and plus its standard deviation: final slope map.
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238 D. Croccolo, R. Cuppini / International Journal of Adhesion & Adhesives 29 (2009) 234–239

Table 3
Characteristics and test values of the four additional tests

Test D% I Mtot (kN m) Mint (kN m) Mad (kN m) Mtest (kN m) Cumulative counts at 4 kN m Slope (cumulative counts/kN m)

V11 1 1 10.04 1.82 8.22 4 22,732 5683

V1.50 1.5 0 10.22 0.09 10.13 4 94,740 23,685
V21 2 1 8.85 1.55 7.30 4 293,888 73,472
V1.52 1.5 2 8.49 3.12 5.37 4 78,524 19,631

Fig. 8. Areas between each slope average minus and plus its standard deviation containing the four additional test slopes.

Table 4
Comparison between the test values and the estimated values of the four additional tests

Test Mtot-real (kN m) Mint (kN m) Mad-real (kN m) Mad-estimateda (kN m) Mtot-estimated (kN m) e% (Mtot)

V11 10.04 1.82 8.22 8.69 10.51 4.4

V1.50 10.22 0.09 10.13 9.88 9.97 2.5
V21 8.85 1.55 7.30 6.89 8.44 4.9
V1.52 8.49 3.12 5.37 5.9 9.02 5.9

a
According to the mathematical model defined in [13].

The AE technique is, therefore, suitable to forecast the defect 5. Conclusion

density of the adhesive and the failure load of the joint with a
good degree of confidence.
In order to verify the non-destructive methodology discussed
above, we performed four additional tests in the same boundary
conditions. All the specimens were loaded until failure in
acquiring the AE and measuring the final releasing moments.
The specimen characteristics, the values of the test results, and
the computed data are presented in Table 3; all the computations
were made in accordance with the methodologies presented in
this paper. The interpolation lines of the four new specimens, as
shown in Fig. 8, stay inside their own area with regard to the
defect density and confirm that the AE technique can be used to
forecast the defect density of the adhesive with a good degree of
confidence.
Finally, the estimated total releasing moments (Mtot) computed
according to [12] were compared to the real ones. The comparison
results reported in Table 4 pointed out a small difference between
the actual values and the estimated ones, with errors always
lower than 6%.
In this paper, the use of AE technique as an NDT one in the field
of adhesively bonded joints is studied in depth. The defect
densities considered are 0%, 25%, 50%, 75% and 100%, while the
interference levels are 0.002, 0.036 and 0.077 mm. The tests have
been performed using some special conical specimens and
according to the DOE method in order to evaluate the presence
and the amount of the adhesive defect density and in order to
define, with accuracy, the map of the cumulative counts slope
variations. The analysis of the AE confirmed the strong correlation
between the maximum load applied and the total cumulative
counts, as well as between the maximum load applied and the
cumulative counts at 4 kN m. The correlation coefficients range
from 0.75 up to 0.96. This strong correlation was verified only for
the same defect density of the adhesive, whereas it does not occur
when the interference level is the same.
The complete map of the slope variations referring to the
cumulative counts of the five adhesive defect densities is reported
in Fig. 6. The area of 25% defect density partially overlaps the 50%
 ARTICLE IN PRESS
D. Croccolo, R. Cuppini / International Journal of Adhesion & Adhesives 29 (2009) 234–239
one; as discussed before, this superposition zone is not repre- References
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[3]
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applying the method to some conical steel joints but it may be [5]
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[11]
and to forecast the value of the releasing moment by comparing [12]
the AE acquired to those uttered by the test specimen; finally, it is [13]
also possible, during the production phase, to decide whether to
discard or to accept the product.
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