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KyungHee Univ.
Surface Modification of Aluminium Powder To
Improve Mechanical Properties of Aluminium
Powder-Polymer Composite.
Part B : Wear-Friction hardness
June 3th, 2011
Jorge Ivan Cifuentes
MECHANICAL ENGINEERING
Nano Composite Lab.
 Introduction
 Wear Mechanism
Nano Composite Lab.
 Experiment
 Aluminium powder 99.7 % from Strem chemicals, U.S.A. The reagents for the
aluminium powder surface modification were pure water J.T. Baker, U.S.A., distilled
water (99.5 %) Dae Jung Chemical (Korea), ethanol (99 % Aldrich, USA) , 3-
aminopropyltriethoxysilane with a purity of 99 % (Aldrich U.S.A.) was used as a silane
functionalization agent.
 The epoxy used was diglycidil ether or Bisphenol A, resin (YD-115, Kukdo Chemical,
Korea) , and the curing agent was polyamidoamine (G-A0533, Kukdo chemicals
Korea).
 Materials & Methods
Nano Composite Lab.
Experiment
Surface Modification of aluminium powder :
- 60 g. of unmodified aluminium powders were dispersed in 250 ml of
ethanol, then 4 ml of APTES dissolved in 25 ml of pure Baker water
was added to the aluminium dispersion
- The aluminium powder and APTES solution was mixed and stirred at 550
rpm for 6 hours at 60 °C.
- After refluxing the solution was filtered with distilled water and acetone
until the ph values approaches 6-7
- Silanized aluminium powders were dried in vaccum oven for 24 hours at
80°C.
 Materials & Methods
Nano Composite Lab.
 Experiment
Epoxy resin was heated at 60 °C and, then 10 % wt of aluminium powder was mixed
within the epoxy by stirring at 400 rpm for 12 hours using a mechanical stirring
-The epoxy resin mixed with hardener (2:1 v/v) were made using 80 g of hardener
added and manually mixed, then poured inside Teflon molds.
-The composite was degassed in a vacuum oven at 760 mm Hg for about 30 min at
room temperature
-- The mold with the composite was kept in an oven and cured at 100 °C for
approximately 15 hours, the it was post cured for 2 hours at 125 °C.
 Materials & Methods
Nano Composite Lab.
 Experiment
Preparation of tensile and fracture specimens:
 The fabricated composites plates were machined as the dog-bone tensile samples,
according to ASTM D 638. Thickness and gage length of the tensile specimens are 5
and 80 mm, respectively.
 Single edge notch specimens (SENT) 4 mm thick18 mm wide a 6 mm initial crack
was prepared for fracture strength toughness measurements.
 Materials & Methods
Nano Composite Lab.
Characterization
 Fourier transform infrared (FTIR) spectra were recorded in unmodified and
silane surface modified aluminium powder and composites on a Jasco
FTIR spectrometer with KBr pellets at a resolution of 4 cm -1 wave
number, in the midinfrared range of 4000 to 400 cm -1 .
 Tensile and fracture tests were performed in an Instron Universal Testing
Machine (Model 8841, Dyna Might) a head rate of 0.2 mm min -1. Fracture
test were performed a head rate of 0.1 mm min -1 . At least 3 specimens of
each composite were tested to ensure reliability of test results.
 The fracture surface of tensile and fracture mode I specimes were studied
by Fiel emission scanning elctron microscope (FE-SEM) (Leo Supra 55,
Carl Zeiss, Germany). The fracture surface were aputered coated with
platinum prior to their observation.
Nano Composite Lab.
Results & Discussion/FTIR
 figure 1 show Characteristic Vibrational
modes (cm-1) , for unmodified and silane surface modified
aluminium powder
a=modified
b=unmodified
Transmitance%
4000 3500 3000 2500 2000 1500 1000
Wave number (cm -1)
Al-OH
Al-O
Si-O-Al
Si-OH-Al
Nano Composite Lab.
Results & Discussion
http://web.khu.ac.kr/~nanocomp/
Company Logo
 Results & Discussion/FTIR
Vibrational mode Unmodified Al
FT-IR
Silanized Al
FT-IR
Unmodified Al-ep
oxy FT-IR
surface modified
Al-epoxy FT-IR
OHstretch(hydroxl ~3400 ---------- ~ 3400 ---------------
(CH2)sym.stretch. -------------- ------------------- ~2848 ~2848
Al-OH ~910 and 3600 ------------ ~3600 ----------------
Si-O-Al ----------- ~1070 ------------- ~1070
C==C stretch ---------------- ~1657 ~1657 - 1713 ~1657 - 1713
Al-O stretch ~900-750 -------------------- --------------------
Si-O-Si(siloxane g) --------------- ~ 1000-1200 -----------------------
-
~1000-1200
Si-OH (Silanol gr.) -------- ~3200-3600 --------------------- ~3200-3600
Table 1. FTIR Characteristic Vibrational modes wavenumber (cm -1) Peak positions and
assignments for unmodified and silane surface modified aluminium powder
Nano Composite Lab.
STRESS -STRAIN
http://web.khu.ac.kr/~nanocomp/
Company Logo
Fig. 2. The elastic modulus was decided by measuring the slope in the
beginning linear region in the stress-strain curve in the elastic area. Is 20
% greater in silane surface modified alumium powder-epoxy composite
Nano Composite Lab.
http://web.khu.ac.kr/~nanocomp/
Company Logo
.
Figure 3 Typical stress-strain curve, in unmodified and
silane surface modified aluminium-epoxy composite
 Tensile Test Results
-10
0
10
20
30
40
50
60
0.25 0.26 0.27 0.28 0.29
Tensilestress(MPa)
Tensile strain (mm/mm)
Specimen 1 to 1
Specimen #
1
Elastic
modulus
0 1 2 3 4
tensile strain (mm/mm) 10 -1
TensileStress(Mpa)
1020304050
modified
unmodified
Nano Composite Lab.
Stress-Strain
http://web.khu.ac.kr/~nanocomp/
Company Logo
Table 2 Tensile stress-strain results of unmodified and silane surface
modified aluminium powder epoxy composite
tensile strength Mpa. Young’s,mo
dulus Gpa.
toughness Elongation- %
Unmodified
Al
38 2 140 3.7
Modified Al 50.10 2.5 210 4.2
Nano Composite Lab.
http://web.khu.ac.kr/~nanocomp/
Company Logo
 Results & Discussion
Figure 3 shows typical tensile stress-strain curves of the Aluminium powder/epoxy
composites with unmodified, ummodified Aluminium powder . As shown in the figure, the
stress increased almost linearly with strain at an early stage, and then nonlinear behavior
occurred before reaching the maximum stress for the both nanocomposites.
 In particular, the tensile strength and Young’s modulus of the Aluminium/epoxy
composites were improved by the silane functionalization. The modified composite
support higher strength , however still is more ductile compare to unmodifed aluminium
powder epoxy composite. Elastic modulus is 20 greater in modified aluminium/epoxy
composite
Nano Composite Lab.
Fracture Results
Fig. 4. Load displacement curve / crack propagation in
fracture test, SENT specimen.
Nano Composite Lab.
Fracture result
http://web.khu.ac.kr/~nanocomp/
Figure 4 shows the comparison of the fracture load and displacement , modified alumium
powder/epoxy composite support 25 % greater fracture load and have 45 % longer
displacement before the collapses .
 As shown in the figure 5, the stress intensity factor Kcr is equal to the fracture
toughness of the material, was calculated by the formula.
KIC = Y Pcr/BW (√a) , where “Pcr” is the fracture strength, “B” is the thickness of the
specimen, “a” is the initial crack length, and Y is the shape function. Table 3 collect the
data of fracture test.
-Fracture toughness is 25 % greater in silane functionalized aluminium powder/epoxy
composite

Nano Composite Lab.
Elastic Modulus
http://web.khu.ac.kr/~nanocomp/
Company Logo
Table 3 . Fracture test result data in surface modified and unmodifed
aluminium/epoxy composite
Fracture load (N) Displacement –du
ctility %
Elastic area ~ resi
lience
Kcr=Fracture tou
ghness
Unmodified Al 408 3.0 29.7 1.53
Modified Al 538 5.55 55.6 2.007
Nano Composite Lab.
http://web.khu.ac.kr/~nanocomp/
Fracture Toughness
figure 5 Fracture Toughness, Mpa √m
Nano Composite Lab.
FESEM
http://web.khu.ac.kr/~nanocomp/
Company Logo
Silane modified unmodified
Figure 6. FESEM on fracture surface of both
composites
Nano Composite Lab.
FESEM
http://web.khu.ac.kr/~nanocomp/
Company Logo
Fig. 6 shown Field emission scaning microscope images
on fracture section on both silane surface modified and
unmodified alumium/epoxy composite.
- Debonding occurs in unmodified alumium/epoxy
composite
-Several microcracks in different direction in silane
surface modified aluminium epoxy composites is
indicating stronger link and adhesion between
aluminium filler and the epoxy matrix, is the reason why
is necessary more energy to break this inter-link and
start the fracture of the composite,
-- opposite occurs in unmodified aluminium epoxy
composite, fracture unidirectional occurs due to weaker
interfacial adhesion between the aluminium filler and the
epoxy matrix..
Nano Composite Lab.
 Conclusions
 This study demonstrated the improved mechanical properties of silane
surface modified aluminium powder epoxy composite
 Silane surface modification of aluminium powder produce better
dispersion in the epoxy matrix and increase the intercalation effect.
Silane alters the hydrophilicity of the of the surface of inorganic
aluminium powder as filler material and improves the adhesion to the
epoxy matrix. The hydrolyzed silane reacts with the hydroxyl from the
aluminium surface by hydrogen bond formation. Then Si-O crosslink are
formed between aluminium surface and the adjacent functional groups in a
condensation rection-elimination of water.
Nano Composite Lab.
http://web.khu.ac.kr/~nanocomp/
 Conclusions
This enhacement is attributed to the good dispersibility and strong
interfacial bonding energy between the functionalized aluminium powder
and the epoxy matrix. It was concluded that the functionalization of
aluminium powder with 3-aminopropyltriethoxysilane is effective in
improving dispersion and adhesion in an epoxy matrix.
Nano Composite Lab.
THANK YOU FOR YOUR
ATTENTION

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Aluminium powder-epoxy composite Wear.

  • 1. KyungHee Univ. Surface Modification of Aluminium Powder To Improve Mechanical Properties of Aluminium Powder-Polymer Composite. Part B : Wear-Friction hardness June 3th, 2011 Jorge Ivan Cifuentes MECHANICAL ENGINEERING
  • 2. Nano Composite Lab.  Introduction  Wear Mechanism
  • 3. Nano Composite Lab.  Experiment  Aluminium powder 99.7 % from Strem chemicals, U.S.A. The reagents for the aluminium powder surface modification were pure water J.T. Baker, U.S.A., distilled water (99.5 %) Dae Jung Chemical (Korea), ethanol (99 % Aldrich, USA) , 3- aminopropyltriethoxysilane with a purity of 99 % (Aldrich U.S.A.) was used as a silane functionalization agent.  The epoxy used was diglycidil ether or Bisphenol A, resin (YD-115, Kukdo Chemical, Korea) , and the curing agent was polyamidoamine (G-A0533, Kukdo chemicals Korea).  Materials & Methods
  • 4. Nano Composite Lab. Experiment Surface Modification of aluminium powder : - 60 g. of unmodified aluminium powders were dispersed in 250 ml of ethanol, then 4 ml of APTES dissolved in 25 ml of pure Baker water was added to the aluminium dispersion - The aluminium powder and APTES solution was mixed and stirred at 550 rpm for 6 hours at 60 °C. - After refluxing the solution was filtered with distilled water and acetone until the ph values approaches 6-7 - Silanized aluminium powders were dried in vaccum oven for 24 hours at 80°C.  Materials & Methods
  • 5. Nano Composite Lab.  Experiment Epoxy resin was heated at 60 °C and, then 10 % wt of aluminium powder was mixed within the epoxy by stirring at 400 rpm for 12 hours using a mechanical stirring -The epoxy resin mixed with hardener (2:1 v/v) were made using 80 g of hardener added and manually mixed, then poured inside Teflon molds. -The composite was degassed in a vacuum oven at 760 mm Hg for about 30 min at room temperature -- The mold with the composite was kept in an oven and cured at 100 °C for approximately 15 hours, the it was post cured for 2 hours at 125 °C.  Materials & Methods
  • 6. Nano Composite Lab.  Experiment Preparation of tensile and fracture specimens:  The fabricated composites plates were machined as the dog-bone tensile samples, according to ASTM D 638. Thickness and gage length of the tensile specimens are 5 and 80 mm, respectively.  Single edge notch specimens (SENT) 4 mm thick18 mm wide a 6 mm initial crack was prepared for fracture strength toughness measurements.  Materials & Methods
  • 7. Nano Composite Lab. Characterization  Fourier transform infrared (FTIR) spectra were recorded in unmodified and silane surface modified aluminium powder and composites on a Jasco FTIR spectrometer with KBr pellets at a resolution of 4 cm -1 wave number, in the midinfrared range of 4000 to 400 cm -1 .  Tensile and fracture tests were performed in an Instron Universal Testing Machine (Model 8841, Dyna Might) a head rate of 0.2 mm min -1. Fracture test were performed a head rate of 0.1 mm min -1 . At least 3 specimens of each composite were tested to ensure reliability of test results.  The fracture surface of tensile and fracture mode I specimes were studied by Fiel emission scanning elctron microscope (FE-SEM) (Leo Supra 55, Carl Zeiss, Germany). The fracture surface were aputered coated with platinum prior to their observation.
  • 8. Nano Composite Lab. Results & Discussion/FTIR  figure 1 show Characteristic Vibrational modes (cm-1) , for unmodified and silane surface modified aluminium powder a=modified b=unmodified Transmitance% 4000 3500 3000 2500 2000 1500 1000 Wave number (cm -1) Al-OH Al-O Si-O-Al Si-OH-Al
  • 9. Nano Composite Lab. Results & Discussion http://web.khu.ac.kr/~nanocomp/ Company Logo  Results & Discussion/FTIR Vibrational mode Unmodified Al FT-IR Silanized Al FT-IR Unmodified Al-ep oxy FT-IR surface modified Al-epoxy FT-IR OHstretch(hydroxl ~3400 ---------- ~ 3400 --------------- (CH2)sym.stretch. -------------- ------------------- ~2848 ~2848 Al-OH ~910 and 3600 ------------ ~3600 ---------------- Si-O-Al ----------- ~1070 ------------- ~1070 C==C stretch ---------------- ~1657 ~1657 - 1713 ~1657 - 1713 Al-O stretch ~900-750 -------------------- -------------------- Si-O-Si(siloxane g) --------------- ~ 1000-1200 ----------------------- - ~1000-1200 Si-OH (Silanol gr.) -------- ~3200-3600 --------------------- ~3200-3600 Table 1. FTIR Characteristic Vibrational modes wavenumber (cm -1) Peak positions and assignments for unmodified and silane surface modified aluminium powder
  • 10. Nano Composite Lab. STRESS -STRAIN http://web.khu.ac.kr/~nanocomp/ Company Logo Fig. 2. The elastic modulus was decided by measuring the slope in the beginning linear region in the stress-strain curve in the elastic area. Is 20 % greater in silane surface modified alumium powder-epoxy composite
  • 11. Nano Composite Lab. http://web.khu.ac.kr/~nanocomp/ Company Logo . Figure 3 Typical stress-strain curve, in unmodified and silane surface modified aluminium-epoxy composite  Tensile Test Results -10 0 10 20 30 40 50 60 0.25 0.26 0.27 0.28 0.29 Tensilestress(MPa) Tensile strain (mm/mm) Specimen 1 to 1 Specimen # 1 Elastic modulus 0 1 2 3 4 tensile strain (mm/mm) 10 -1 TensileStress(Mpa) 1020304050 modified unmodified
  • 12. Nano Composite Lab. Stress-Strain http://web.khu.ac.kr/~nanocomp/ Company Logo Table 2 Tensile stress-strain results of unmodified and silane surface modified aluminium powder epoxy composite tensile strength Mpa. Young’s,mo dulus Gpa. toughness Elongation- % Unmodified Al 38 2 140 3.7 Modified Al 50.10 2.5 210 4.2
  • 13. Nano Composite Lab. http://web.khu.ac.kr/~nanocomp/ Company Logo  Results & Discussion Figure 3 shows typical tensile stress-strain curves of the Aluminium powder/epoxy composites with unmodified, ummodified Aluminium powder . As shown in the figure, the stress increased almost linearly with strain at an early stage, and then nonlinear behavior occurred before reaching the maximum stress for the both nanocomposites.  In particular, the tensile strength and Young’s modulus of the Aluminium/epoxy composites were improved by the silane functionalization. The modified composite support higher strength , however still is more ductile compare to unmodifed aluminium powder epoxy composite. Elastic modulus is 20 greater in modified aluminium/epoxy composite
  • 14. Nano Composite Lab. Fracture Results Fig. 4. Load displacement curve / crack propagation in fracture test, SENT specimen.
  • 15. Nano Composite Lab. Fracture result http://web.khu.ac.kr/~nanocomp/ Figure 4 shows the comparison of the fracture load and displacement , modified alumium powder/epoxy composite support 25 % greater fracture load and have 45 % longer displacement before the collapses .  As shown in the figure 5, the stress intensity factor Kcr is equal to the fracture toughness of the material, was calculated by the formula. KIC = Y Pcr/BW (√a) , where “Pcr” is the fracture strength, “B” is the thickness of the specimen, “a” is the initial crack length, and Y is the shape function. Table 3 collect the data of fracture test. -Fracture toughness is 25 % greater in silane functionalized aluminium powder/epoxy composite 
  • 16. Nano Composite Lab. Elastic Modulus http://web.khu.ac.kr/~nanocomp/ Company Logo Table 3 . Fracture test result data in surface modified and unmodifed aluminium/epoxy composite Fracture load (N) Displacement –du ctility % Elastic area ~ resi lience Kcr=Fracture tou ghness Unmodified Al 408 3.0 29.7 1.53 Modified Al 538 5.55 55.6 2.007
  • 17. Nano Composite Lab. http://web.khu.ac.kr/~nanocomp/ Fracture Toughness figure 5 Fracture Toughness, Mpa √m
  • 18. Nano Composite Lab. FESEM http://web.khu.ac.kr/~nanocomp/ Company Logo Silane modified unmodified Figure 6. FESEM on fracture surface of both composites
  • 19. Nano Composite Lab. FESEM http://web.khu.ac.kr/~nanocomp/ Company Logo Fig. 6 shown Field emission scaning microscope images on fracture section on both silane surface modified and unmodified alumium/epoxy composite. - Debonding occurs in unmodified alumium/epoxy composite -Several microcracks in different direction in silane surface modified aluminium epoxy composites is indicating stronger link and adhesion between aluminium filler and the epoxy matrix, is the reason why is necessary more energy to break this inter-link and start the fracture of the composite, -- opposite occurs in unmodified aluminium epoxy composite, fracture unidirectional occurs due to weaker interfacial adhesion between the aluminium filler and the epoxy matrix..
  • 20. Nano Composite Lab.  Conclusions  This study demonstrated the improved mechanical properties of silane surface modified aluminium powder epoxy composite  Silane surface modification of aluminium powder produce better dispersion in the epoxy matrix and increase the intercalation effect. Silane alters the hydrophilicity of the of the surface of inorganic aluminium powder as filler material and improves the adhesion to the epoxy matrix. The hydrolyzed silane reacts with the hydroxyl from the aluminium surface by hydrogen bond formation. Then Si-O crosslink are formed between aluminium surface and the adjacent functional groups in a condensation rection-elimination of water.
  • 21. Nano Composite Lab. http://web.khu.ac.kr/~nanocomp/  Conclusions This enhacement is attributed to the good dispersibility and strong interfacial bonding energy between the functionalized aluminium powder and the epoxy matrix. It was concluded that the functionalization of aluminium powder with 3-aminopropyltriethoxysilane is effective in improving dispersion and adhesion in an epoxy matrix.
  • 22. Nano Composite Lab. THANK YOU FOR YOUR ATTENTION