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Microindentation characterization of polymers and polymer based
nanocomposites
V. Lorenzo
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• Hardness and hardness measurement
– Vickers hardness
– Relationships between hardness and other mechanical properties of polymers
– DSI
– Microindentation and viscoleasticity
• Microhardness of heterogeneous polymer systems
– Microhardness of semycrystalline polymers
– Microhardness of blends
– Microhardness and physical ageing
– Microhardness of PMC's
– Microhardness of PMnC's
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Microindentation of polymersMay 2011
Hardness
• DEFINITION: a measure of the resistance to permanent surface deformation or damage.
– Local character of measurement
– What is the meaning of surface damage?
• METHODS OF TESTING:
– Scratching
– Static indentation
– Dynamic indentation
– ...
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• Hardness and hardness measurement
– Vickers hardness
– Relationships between hardness and other mechanical properties of polymers
– DSI
– Microindentation and viscoleasticity
• Microhardness of heterogeneous polymer systems
– Microhardness of semycrystalline polymers
– Microhardness of blends
– Microhardness and physical ageing
– Microhardness of PMC's
– Microhardness of PMnC's
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Microindentation of polymersMay 2011
The Vickers test
• Static penetration test
• Diamond square based pyramidal indentor (angle between the faces: 136º)
– Diamond: indentor remains undeformed during the test
– Pyramidal: geometric similarity of indentations ⇒ hardness is load independent
– 136º: HV ≈ HB if HB < 600
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Microindentation of polymersMay 2011
Stages of the test
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Microindentation of polymersMay 2011
Stages of the test
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Microindentation of polymersMay 2011
Stages of the test
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Microindentation of polymersMay 2011
Vickers hardness definition
• Average pressure on the lateral surface of the residual indentation
• HYP.: the geometries of indentor and indentation are similar ⇒
– h = d/7 and Slat = d2/(2.sin 68º)
d: diagonal of the base of the residual imprint
h: indentation depth; Slat
: contact area
– HV = 2.sen 68º P/d2
HV: Vickers hardness; P: load
• MICROHARDNESS: hardness measured after applying small loads (grams) ⇒ diagonal of the residual indentation: µm
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Microindentation of polymersMay 2011
Stress distribution under the indentor
• Classical results and FEM calculations:
– Stresses are confined to a hemispherical region with radius ≈1,5d≈10h
• Some practical considerations:
– Minimal distance between two indentations
– Minimal distance between indentations and edges
– Minimal thickness of films
– Very small sample quantity (ng)
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• Hardness and hardness measurement
– Vickers hardness
– Relationships between hardness and other mechanical properties of polymers
– DSI
– Microindentation and viscoleasticity
• Microhardness of heterogeneous polymer systems
– Microhardness of semycrystalline polymers
– Microhardness of blends
– Microhardness and physical ageing
– Microhardness of PMC's
– Microhardness of PMnC's
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Microindentation of polymersMay 2011
Relationships between MH and other mechanical properties
V. Lorenzo et al.: Die Ang. Makromol. Chem., 172 (1989) 25-35
V. Lorenzo et al.: J. Mater. Sci. Let., 8 (1989) 1455-1457
J. Arranz et al.: Polymer, 46 (2005) 12287-12297
Palza, H. et al.: Macromol. Chem. Phys., 209 (2008) 2259-2267
V.Lorenzo et al.: communication to EPF2011, Granada, 26th June-1st July
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Microindentation of polymersMay 2011
Relationships between MH and other mechanical properties
V. Lorenzo et al.: Die Ang. Makromol. Chem., 172 (1989) 25-35
V. Lorenzo et al: J. Mater. Sci. Let., 8 (1989) 1455-1457
G. Zamfirova et al.: J. Appl. Polym. Sci., 88 (2003) 1794-1798
J. Arranz et al.: Polymer, 46 (2005) 12287-12297
Palza, H. et al.: Macromol. Chem. Phys., 209 (2008) 2259-2267
V.Lorenzo et al.: communication to EPF2011, Granada, 26th June-1st July
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• Hardness and hardness measurement
– Vickers hardness
– Relationships between hardness and other mechanical properties of polymers
– DSI
– Microindentation and viscoleasticity
• Microhardness of heterogeneous polymer systems
– Microhardness of semycrystalline polymers
– Microhardness of blends
– Microhardness and physical ageing
– Microhardness of PMC's
– Microhardness of PMnC's
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Microindentation of polymersMay 2011
DSI: Depth Sensing Indentation
• 1980's: continuous measurements of load and indentation depth
• Very small loads (mN) ⇒ resolution: µN
• Very small indentation depths (tenths of µm) ⇒ resolution: nm
• Berkovich indenterFischer Cripps, A.: 'Nanoindentation',
Springer (2004)
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Microindentation of polymersMay 2011
Results of DSI tests
• Hardness under load
• Creep
• Elastic modulus
• Delayed elastic recovery
• Deformation energy
• Recoverable energy
• …
• And, of course, hardness
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• Hardness and hardness measurement
– Vickers hardness
– Relationships between hardness and other mechanical properties of polymers
– DSI
– Microindentation and viscoleasticity
• Microhardness of heterogeneous polymer systems
– Microhardness of semycrystalline polymers
– Microhardness of blends
– Microhardness and physical ageing
– Microhardness of PMC's
– Microhardness of PMnC's
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Microindentation of polymersMay 2011
Geometry of the residual indentations on polymers
V.Lorenzo et al.: J. Mater. Sci., 23 (1988) 3168
100 h(t)/d = α + β exp(-t/τ)
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Microindentation of polymersMay 2011
Delayed elastic recovery studyby means of DSI measurements
V.Lorenzo et al.: communication to EPF2011, Granada, 26th June-1st July
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Microindentation of polymersMay 2011
Creep study by means of DSI measurements
• Model:
V.Lorenzo et al.: communication to EPF2011, Granada, 26th June-1st July
Q 410 0,48 23S 675 0,46 18
Sample E (MPa) τ (s) Cit (%)
h2 t =2
P0cotg[ 1E1
1E2 1−expE2 t
2 t1 ]
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Microindentation of polymersMay 2011
Delayed elastic recovery studyby means of DSI measurements
Model:
h(t) = h(0) + A(1 – exp(-t/τ))
• Retardation time, τ, structure independent
• Not a quantitative agreement
– Interferometry experiments
• Indenter geometry
• Sampling frequency
– Creep results:
• Non linearity
V.Lorenzo et al.: communication to EPF2011, Granada, 26th June-1st July
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• Hardness and hardness measurement
– Vickers hardness
– Relationships between hardness and other mechanical properties of polymers
– DSI
– Microindentation and viscoleasticity
• Microhardness of heterogeneous polymer systems
– Microhardness of semycrystalline polymers
– Microhardness of blends
– Microhardness and physical ageing
– Microhardness of PMC's
– Microhardness of PMnC's
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Microindentation of polymersMay 2011
Local character of the measurement
• Microindentation “averages” the properties of some µm3 of the material around the indentor.
• Microindentation and heterogeneity of the specimen:
– Characteristic length of heterogeneities > d ⇒ MH = f(x, y)• Information about distribution of phases• Characterization of phases
– Characteristic length of heterogeneities < d ⇒ MH is not a function of the position
• Bulk properties of the material
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• Hardness and hardness measurement
– Vickers hardness
– Relationships between hardness and other mechanical properties of polymers
– DSI
– Microindentation and viscoleasticity
• Microhardness of heterogeneous polymer systems
– Microhardness of semycrystalline polymers
– Microhardness of blends
– Microhardness and physical ageing
– Microhardness of PMC's
– Microhardness of PMnC's
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Microindentation of polymersMay 2011
Microhardness and crystallinity of polymers
• Polyethylenes that has been quickly cooled form the melt:
– Length of crystallites < d ⇒ MH is not a function of the position ⇒ MH is an increasing function of crystallinity level
– Information about deformation mechanism
V. Lorenzo et al.: Die Ang. Makromol. Chem., 172 (1989) 25-35
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Microindentation of polymersMay 2011
Properties of the phases of semycrystalline polymers
• It is not possible to obtain a 100% crystalline or amorphous PE sample.
• Mechanical properties of phases can be obtained by extrapolating MH measurements
Baltá-Calleja, F.J.; Fakirov, S., 'Microhardness of Crystalline Polymers' ; Cambridge University Press: Cambridge, 2000
• Isothermally crystallized iPP displays spherulites of the α and β polymorphs ⇒ properties of the α and β spherulites
Seidler, S.: JOURNAL OF MACROMOLECULAR SCIENCE, Part B—Physics, B41 (2002) 851–861
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• Hardness and hardness measurement
– Vickers hardness
– Relationships between hardness and other mechanical properties of polymers
– DSI
– Microindentation and viscoleasticity
• Microhardness of heterogeneous polymer systems
– Microhardness of semycrystalline polymers
– Microhardness of blends
– Microhardness and physical ageing
– Microhardness of PMC's
– Microhardness of PMnC's
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Microindentation of polymersMay 2011
Microhardness of blends
• Blends of miscible A and B polymers:homogeneous at d scale ⇒ MH = f(%A)
• Blends of inmiscible A and B polymers: separated domains of A and B
– If %A << %B ⇒ characteristic length of A domains < d ⇒ MH is a continuous function of %A
• Continuity of MH(%A) miscibility
– If %A is comparable con %B:
• Characteristic length of A domains < d
• Characteristic length of A domains > d– MH is a function of the position– Characterization of individual phases
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Microindentation of polymersMay 2011
V. Lorenzo et al.: J. Mater. Sci. Lett., 9 (1990) 1011-1013
Microhardness of blends of PEO with iPMMA
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Microindentation of polymersMay 2011
Microhardness of blends of polyolefins and LCP's
J. Arranz et al.: doi:10.1016/j.memsci.2011.04.023
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• Hardness and hardness measurement
– Vickers hardness
– Relationships between hardness and other mechanical properties of polymers
– DSI
– Microindentation and viscoleasticity
• Microhardness of heterogeneous polymer systems
– Microhardness of semycrystalline polymers
– Microhardness of blends
– Microhardness and physical ageing
– Microhardness of PMC's
– Microhardness of PMnC's
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Microindentation of polymersMay 2011
Microhardness and physical ageing
• A – Tg: liquid
– Cooperative movement of chains
• Tg – B: glass
– Movements of local groups
• B – C: physical ageing
– Densification:
• Local free volume fluctuations
• Correlation length < 10-1 μm
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Microindentation of polymersMay 2011
Physical ageing of LCP's and SMP's as revealed by MH tests
V. Lorenzo et al.: Materials and Design 30 (2009) 2431–2434
A. Ormazábal et al. In “Nanostructured and Non-Crystalline Materials”, World Scientific, Singapore (1995) 202-206
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• Hardness and hardness measurement
– Vickers hardness
– Relationships between hardness and other mechanical properties of polymers
– DSI
– Microindentation and viscoleasticity
• Microhardness of heterogeneous polymer systems
– Microhardness of semycrystalline polymers
– Microhardness of blends
– Microhardness and physical ageing
– Microhardness of PMC's
– Microhardness of PMnC's
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Microindentation of polymersMay 2011
Microhardness of polymeric matrix composites
• Composites are multiphasic materials: fillers dimesions ~ some tens of µm ⇒ characteristic dimensions of heterogeneities > d ⇒ MH is position function ⇒ MH is not an adequate tool for characterizing composite materials
But it can be used for:
– Characterizing matrix and fillers.
– Characterizing interphases:• Transcrystalline structures in GF reinforced PP composites
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• Hardness and hardness measurement
– Vickers hardness
– Relationships between hardness and other mechanical properties of polymers
– DSI
– Microindentation and viscoleasticity
• Microhardness of heterogeneous polymer systems
– Microhardness of semycrystalline polymers
– Microhardness of blends
– Microhardness and physical ageing
– Microhardness of PMC's
– Microhardness of PMnC's
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Microindentation of polymersMay 2011
Microhardness of nanocomposites
• Aglommerated fillers:
– characteristic length of heterogeneities > d ⇒ MH is a function of position
• If the fillers are well dispersed:
– characteristic length of heterogeneities < d ⇒ MH = f(% filler) ⇒ information about the reinforcement effect of the filler.
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Microindentation of polymersMay 2011
PC-clay nanocomposites obtained by disolution
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Microindentation of polymersMay 2011
Other heterogeneous polymeric materials
• Characterization of coatings
• Multi-layer extrusion
• Skin-core structures in injection molded polymers
• Composition gradients
• ...
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Microindentation of polymersMay 2011
Summarizing
• Microindentation is an adequate tool for exploring structure of polymeric materials
• The volume of material that is deformed in hardness test is around d3
• The information that can be obtained from a hardness test depends on the characteristic length of the heterogeneities of the sample, l:
– If l < d, bulk porperties of the material
– If l > d, local character information
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The research group
• ICTP (CSIC)
– Prof. J.M. Pereña
– Prof. R. Benavente
– Prof. E. Pérez
– Prof. M.L. Cerrada
– Dr. J. Arranz
• ETSII (UPM)
– Prof. J. Martínez
– Prof. De la Orden
– Prof. G. Pinto
– Prof. V. Lorenzo
and all the postdoc, students and technicians that have collaborated with us.
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Microindentation of polymersMay 2011
Thank you very much for your attention
Merci pour votre attention
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