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16
1999 InternationalSymposium on Advanced Packaging Materials
17
1999 International Symposium on Advanced Packaging Materials
quantifying the signifkantly small levels of organic on the surfaces. In the case of both oleic acid and
material present. Secondly, assuming the organic stearic acid shown in Table 1, the amount of material
material is all lubricant, this information can be used present is consistent with films of molecular
along with estimated surface areas to give an dimensions (monolayer or bilayer).
indication of the thickness of the lubricant adsorbed
None 0.03
Oleic Acid 0.10
I Stearic Acid I 0.29 I
-- I I
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1999 International Symposium on Advanced Packaging Materials
Figure 5. Oleic Acid Lubricated Silver Subjected to Figure 7.90" Cls X P S Spectrum
Multiple Heating Cycles
- M
41
-I -T m ..tu-
I: ~i
3.5 Diffise Reflectance Infrared Suectroscouv
(DRIR) Results
The occurrence of the exotherm suggests that the Further evidence of chemical bonding is given in the
reaction occurring involves a chemical change on the vibrational spectra. DRIFTS spectra of a lubricant
silver surface rather than a change in the state of adsorbed to silver flakes is given in Figure 9. The
lubricant. However, the temperature dependence of presence of a strong peak centered around 1398 cm-'
the exotherm on the lubricant type suggests that can be assigned to the [0-C-01 symmetric stretch [4],
lubricant binding inhibits the exothermic reaction which suggests that a sigmkant amount of the
that occurs and therefore would have an activation lubricant is forming a salt with the silver surface.
energy that is lubricant dependent. Related studies The virtual absence of any intensity around 1700 cm-
have suggested that the exotherm corresponds to a for the C=O stretch of the acid dimer suggests that
combination of oxidation of the silver surface andor all the acid functionality on the Ag surface was
oxidation of the lubricant [3]. modified.
3.4 X-ray Photoelectron Suectroscoov (XPS)Results Figure 9. DRIFT Spectrum of Oleic Acid Lubricated
Silver Flake
XPS data also supports the presence of the lubricant
only at molecular dimensions, specifically
monolayer. Both the Cls, (Figure 7), and Ols, I
(Figure 8), spectra for all the samples showed no sign I NglsilWpatids
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1999 International Symposium on Advanced Packaging Materials
3.6 Raman SpectroscoDy the silver flakes is possible with the DRIFTS and
Raman spectra. The DRIFTS spectra clearly shows
Further evidence for lubricant bonding to the silver the presence of the 0-C-0 in the form of a symmetric
surface comes from the Raman spectrum of the stretch. In the Raman spectrum, the same symmetric
treated powders. Spectra in Figure 10 show that the stretch peak is observed. In addition, the spectra
[O-C-01 symmetric stretch peak appears around suggests the presence of a small amount of oleic acid
1395 cm- [5]. In addition, the 1609 cm- is likely (C=C stretch) as a contaminant.
due to a C= stretch coordinated with the silver
surface for a small amount of oleic acid which is 5. References
usually found in stearic acid.
1. Y. Iwasa et al., Conductive Adhesive for Sui$ace
Figure 10. Raman Spectrum of Stearic Acid Mount Devices, Electronic Packaging &
Lubricated Silver Compared with Neat StearicAcid Production, pp. 93-98, Nov. 1997.
2. U.S. Patent, 5,413,617, Process for the
Preparation of Sliver Powder with a
Controlled Surface Area by Reduction
Reaction.
3. D. Lu et al., A Fundamental Study on Silver
Flakes for Conductive Adhesives4th
M A P S Proceedings, Braselton, Georgia,
15-18 March 1998, U.S.A., pp. 256-260.
4. H. Han et al., D i m e Reflectance Infiared
Spectra of 4-Nitrobenzioc Acid and 4-
Cyanobenzoic Acid Self-Assembled on Fine
Silver Particles, Applied Spectroscopy, vol.
52, n. 8, 1998.
5. Dollish, Francis R.; Fateley, William G.;
Bentley, Freeman F.; Characteristic Raman
Frequencies of Organic Compounds, 1974,
John Wiley and Sons,Inc., New York.
4. Conclusion:
Overall, the data suggest that acid lubricants form
stable monolayers chemically bonded to the silver
surfaces. The effect is shown in the ultimate
morphology and physical properties. These physical
and morphological properties can be related to the
rheological properties previously shown for SMCAs.
The SEM data show that ball milling with lubricants
gives a completely different morphology of silver
particles versus not lubricating the particle at all. It
also shows that the presence of lubricant reduces the
clustering of silver particles.
The DSC results indicate that the lubricant is
chemically bonded to the silver powders. The
temperature dependence of the exothermic peak may
be a consequence of the chemical binding. The
exothermic process does not likely occur untd after
the lubricant is debonded from the surface during the
heating process and may be due to either lubricant or
silver oxidation at the elevated temperatures.
X P S data confirms the presence of carbon and
oxygen at levels consistent with oleic acid. In
addition, the spectra also suggests that the oleic acid
is bonding to the silver surface as a salt. The virtual
absence of free acid in the X P S data indicates that the
lubricant is present as a monolayer.
Direct observation of the change in the state of the
stearic acid from the solid state to the monolayer on
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