Applications

Optical microscopy


Indenter positioning – displacement between microscope focus point and indenter tip is calibrated with 1 um accuracy

Measuring linear size (and area) over the optical image

Example: coated cutting tools

	Sample: micro-drill for electronics industry applications	R_a = 70 nm RMS = 86 nm R_z = 232 nm H = 30,8±6,5 GPa E = 675±105 GPa k = 2,15±0,05 kN/m


Sample: cutting edge of the fraise	Surface topography	Image of the residual imprint

Example: multilayer coating on cutting tools


Sample	Sample angle polish	Optical image of layered structure

Material	Hardness, GPa	Elastic modulus, GPa
Hard Alloy	19.0 ± 5.4	410 ± 140
TiCN	17.7 ± 4.5	340 ± 80
Al₂O₃	20.4 ± 4.0	340 ± 35
TiN	10.9 ± 3.3	360 ± 200

Localized nanomechanical tests


Topography: before indentation	Topography: after indentation

Sample: aluminum alloy D16

SPM aids indentation: pile-up analysis

Pile-up analysis on steel 254 reference block HV 0.05

X – rheological factor

E – Young’s modulus

ρ₀ – yield stress

θ – semi-apical angle of indenter

Study of delamination, adhesion and thickness

Sample: plasma sputtered diamond-like coating

	Thickness, nm	Load at which film is pulled, mN
1	460 ± 20	6,2 ± 0,3
2	265 ± 10	5,9 ± 0,3
3	960 ± 70	11,0 ± 2,6
4	1255 ± 20	20,8 ± 6

Reciprocating wear tests

Spherical Al₂O₃ tip

Sample	∆h, nm
Duralumin (untreated)	75 ± 15
Duralumin with protective mineral coating	5.9 ± 1.2

Wear estimation of coatings

Wear time diagram	Indirect volume estimation over the optical micro-photograph of the groove


J = (L×t×ν)/h	R=17 um — effective stylus radius; w — width of the residual groove; L=100 um — groove length;
L=100 um — stroke length; ν=0,13 Hz — reciprocating test frequency; t=7600 sec — testing time; h — indentor penetration depth;	Direct volume estimation over the SPM image

ABI (automated ball indentation)

		Experimental multicycle loading-unloading curves

2D: H=f(x, y), static loading

Sample: gradient magnetic alloy of the following composition:

Chemical element	Cr	Ni	Si	Mn	C	V	Fe
Contents, %	16,5	7,5	0,48	1,0	0,08	0,04	remains


Hardness map of the magnetic zone boundary
	Hardness profile across the magnetic zone boundary

Mapping 3D: H=f(x, y, z), hardness tomography

Volumetric quantitative map Optical micro-photo of the array of PUL indentations
	Volumetric quantitative map (tomogram) of hardness

Mapping 3D: hardness tomography

Sample: separation border between copper and Fe-Cr-Al alloy

Sample: Polymer material for tooth prosthetics

	It has been shown that chemical treatment reduces hardness and elastic modulus for 10-15% Blue lines – before treatment Green lines – after treatment

Surface topography and cross-section profile	Hardness vs. depth dependency for 3 polymer samples	Elastic modulus vs. depth dependency for 3 polymer samples

Sample: Thin film of poly-n-isopropylacrylamide

This polymer exhibits the properties of superabsorbent and is used in pharmaceutical industry during remedies extraction.

Thickness, nm	Hardness, GPa
100	0.5 ± 0.1
5000	1.1 ± 0.3

Height profile of the pNIPAm film. Pile up effect depends on applied forces (F) and film thickness (h): a) F=5mN, h=5µm; b) F=1mN, h=100nm; c) F=2mN, h=100nm.

Example: protective polymer coatings

Samples: polymer materials with thermosetting siloxane protective coating

Profile, hardness, elastic properties testing

Polycarbonate (1)

Polymethylmethacrylate (2)

Polycarbonate + coating (3)

Instrumented indentation loading-unloading curves

Sample	Roughness, nm	Elastic (Young) modulus, GPa	Hardness, GPa	Elastic recovery rate, %
PC	11,8	2,2	0,27	72
PMMA	4,4	4,5	0,33	60
PC+coating	0,5	1,4	0,68	99

Topography image after progressive scratch test (0 to 30 mN): PC (a) and PC+coating (b)

Mapping 2D: H=f(x, y), dynamic loading

Sample: glass fibers in the polymer matrix


Surface topography	Hardness map
	F - load force, Δf - shift of the resonance frequency, f₀ - the resonance frequency of free probe k - the dynamic stiffness. Using this formula allows us to calculate H/E² (and accordingly, H or E if at least one of these quantities is known) as a function of depth or surface coordinates.

Mapping 3D: hardness tomography

Sample: transition area between 2 polymer coatings on polydimethilsiloxane (PDMS) substrate


Hardness tomography technique is based on combination of PUL or DMA method with precise indentor positioning over the regular XY grid on the sample surface

Samples: polyethylene multilayer film with thickness 50-300 um

Task: testing the mechanical strength and resistance to puncture of films on the

substrates of polypropylene and steel



Loading-unloading curves obtained with Berkovich diamond indentor	Loading curves during puncture test with flat punch indentor showing comparison of mechanical strength of polymer films

NIOS Nanomechanical Testers: Metal-ceramic and polymer applications

Optical microscopy

Example: coated cutting tools

Example: multilayer coating on cutting tools

Localized nanomechanical tests

Sample: aluminum alloy D16

SPM aids indentation: pile-up analysis

Study of delamination, adhesion and thickness

Sample: plasma sputtered diamond-like coating

Reciprocating wear tests

Wear estimation of coatings

ABI (automated ball indentation)

2D: H=f(x, y), static loading

Mapping 3D: H=f(x, y, z), hardness tomography

Mapping 3D: hardness tomography

Sample: Polymer material for tooth prosthetics

Sample: Thin film of poly-n-isopropylacrylamide

Example: protective polymer coatings

Mapping 2D: H=f(x, y), dynamic loading

Mapping 3D: hardness tomography

Samples: polyethylene multilayer film with thickness 50-300 um

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