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Hot nanoindentation in inert environments
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10.1063/1.3436633
/content/aip/journal/rsi/81/7/10.1063/1.3436633
http://aip.metastore.ingenta.com/content/aip/journal/rsi/81/7/10.1063/1.3436633

Figures

Image of FIG. 1.
FIG. 1.

The interplay between temperature and indentation scale established by previous nano- and microindentation (differentiated with circles and squares, respectively) at elevated temperatures (Refs. 3, 5, 8, and 10–46). Two regions are identified: one that is defined by indentation on nonoxidizing materials and a second, much smaller regime that is defined by metals alone (open symbols). To expand the second regime, minimization of thermal drift and sample oxidation are required.

Image of FIG. 2.
FIG. 2.

Schematic of (a) the nanoindenter integrated with the vacuum chamber and heating and cooling systems. (b) is an expanded view of the dashed box in (a) which includes the indenter assembly (e.g., piezotube and transducer), actively cooled transducer shield, and the heater cartridge. (c) is a schematic of the tip engaged with the sample [highlighted by the dashed box in (b)] and its dimensions.

Image of FIG. 3.
FIG. 3.

Representative load-displacement curves recorded on fused silica at 23, 320, and in vacuum with a Berkovich diamond tip attached to a standard Macor shaft. The unload drift is measured by holding at load during unloading for 10 s. The recorded displacement (indicated by arrows) is the drift, which increases with temperature. The larger arrow indicates the direction we define as positive drift.

Image of FIG. 4.
FIG. 4.

Drift rates measured during preloading and unloading as a function of indentation time. Each point on the graphs is taken from a single indentation.

Image of FIG. 5.
FIG. 5.

Average steady state drift rates as a function of temperature measured using (a) different tip architectures in vacuum and (b) in different inert atmospheres using a tip with a standard Macor shaft (without a secondary shield). The error bars represent one standard deviation. The “(u)” and “(p)” demarcations next to each data label indicate whether the drift rate is unload or preload, respectively. Data for “air” in (b) are extracted from Ref. 33.

Image of FIG. 6.
FIG. 6.

Displacement as a function of time of a tip assembly (diamond tip with a Macor shaft) during unload and preload holds in several materials as calculated by the model presented here. (a) The calculated displacements during a preload and unload hold in fused silica. The inset table displays the measured and calculated preload and unload drift rates for comparison in both fused silica and Cu. (b) The calculated displacements during an unload hold in fused silica and Cu. The inset table displays the measured and calculated unload drift rates for several materials tested.

Image of FIG. 7.
FIG. 7.

Noise (standard deviation of the average drift rates) as a function of temperature (a) using different tip architectures in vacuum and (b) using a tip with a Macor shaft in different inert atmospheres. The (u) and (p) demarcations next to each data label indicate whether the noise is related to the unload or preload drift rate, respectively. Data for air in (b) are extracted from Ref. 33.

Image of FIG. 8.
FIG. 8.

Load-displacement curves (corrected for drift using unloading drift) recorded in fused silica at various temperatures using a diamond tip attached to a zero thermal expansion shaft. Indentations recorded at 23 and are consistent with the changes in hardness and reduced modulus. A significant change in the shape of the curve is observed at , and this change persists after cooling to .

Image of FIG. 9.
FIG. 9.

(a) Hardness and (b) reduced modulus of fused silica as a function of temperature measured by nanoindentation. For the present work, measurements were done in vacuum with a diamond tip attached to a zero thermal expansion shaft. Each data point represents more than 50 indentations each with the error bars being the standard deviations of those averages. For comparison, similar data recorded in air by Schuh and co-workers (Ref. 33) and Beake and Smith (Ref. 24) are also shown.

Image of FIG. 10.
FIG. 10.

(a) Hardness and (b) reduced modulus of annealed Al (99.998% pure) as a function of temperature measured by nanoindentation. For the present work, measurements were done in Ar near atmospheric pressure with a diamond tip attached to a zero thermal expansion shaft. Each data point represents the average of more than 20 indentations each with the error bars being the standard deviations of those averages. For comparison, hardness values collected using nanoindentation (Ref. 23) and hot microhardness (Refs. 48, 66, and 67) are also shown in (a). Reduced modulus data in (b) is compared to that calculated from acoustic data (Refs. 68–73).

Image of FIG. 11.
FIG. 11.

(a) Hardness and (b) reduced modulus of annealed Cu (99.95% pure) as a function of temperature measured by nanoindentation. For the present work, measurements were done in Ar near atmospheric pressure with a diamond tip attached to a zero thermal expansion shaft. Each data point represents the average of more than 20 indentations each with the error bars being the standard deviations of those averages. Hardness values in (a) are compared to hot hardness data (Refs. 66, 67, and 76–79, while reduced modulus values in (b) are compared to that calculated from acoustic data (Refs. 68, 70, and 80–86).

Tables

Generic image for table
Table I.

Sample materials indented at and the measured unload drift rates. The drift rate increases with the thermal conductivity of the sample material.

Generic image for table
Table II.

Loading conditions and unload drift rates for measurements of material properties.

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/content/aip/journal/rsi/81/7/10.1063/1.3436633
2010-07-01
2014-04-18
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752b84549af89a08dbdd7fdb8b9568b5 journal.articlezxybnytfddd
Scitation: Hot nanoindentation in inert environments
http://aip.metastore.ingenta.com/content/aip/journal/rsi/81/7/10.1063/1.3436633
10.1063/1.3436633
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