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Low Temperature Nanoindentation: Development and Applications

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Low Temperature Nanoindentation: Development and Applications micromachines Review Low Temperature Nanoindentation: Development and Applications Shunbo Wang 1 and Hongwei Zhao 1,2,* 1 School of Mechanical and Aerospace Engineering, Jilin University, Changchun 130025, China; [email protected] 2 Key Laboratory of CNC Equipment Reliability, Ministry of Education, Changchun 130025, China * Correspondence: [email protected]; Tel.: +86-0431-85095757 Received: 15 March 2020; Accepted: 30 March 2020; Published: 13 April 2020 Abstract: Nanoindentation technique at low temperatures have developed from initial micro-hardness driving method at a single temperature to modern depth-sensing indentation (DSI) method with variable temperatures over the last three decades. The technique and implementation of representative cooling systems adopted on the indentation apparatuses are discussed in detail here, with particular emphasis on pros and cons of combination with indentation technique. To obtain accurate nanoindentation curves and calculated results of material properties, several influence factors have been carefully considered and eliminated, including thermal drift and temperature induced influence on indenter and specimen. Finally, we further show some applications on typical materials and discuss the perspectives related to low temperature nanoindentation technique. Keywords: low temperature; nanoindentation; hardness test; apparatus; mechanical properties 1. Introduction Nanoindentation technique has become one of the most popular mechanical property testing methods in recent years [1–5]. Compared with uniaxial tension and compression tests, the specimen requirements of nanoindentation were more simplified: a flat, no shape required surface. The mechanical properties, including but not limited to hardness and elastic modulus, can be obtained automatically via commercial system using Hertz contact theory [6] and Oliver-Pharr analysis method [7]. Moreover, selectable micro-region and huge testing amount on the single specimen provides significant advantages of nanoindentation over other macro-mechanical tests. Mechanical properties of each component of the specimen can be studied separately in details, as well as the interaction between them [8,9]. The negligible testing area of nanoindentation is also in favor of high throughput test and testing on small-scale materials, such as films and particles [10,11]. With attaching low temperature environment on the conventional nanoindentation system, materials can be investigated at service temperatures and conditions relevant to industrial applications via nanoindentation method. Scientifically, low temperature nanoindentation technique is attractive to academic researchers for its combination low temperature environment to convenient nanoindentation method. The researchable aspects are not only limited to variation of specific mechanical parameters with temperature decreasing, while high hydrostatic pressure, shear stress, and local strain can be easily realized via nanoindentation method [12–14]. Interesting phenomena caused by such reasons are also strongly associated with the variation of temperature. Combining with subsequent testing analysis procedures on residual impressions, such as focused ion beam (FIB), scanning electron microscope (SEM), and transmission electron microscope (TEM) methods, the complex evolvement caused by nanoindentation at low temperatures can be observed intuitively [15–18]. Micromachines 2020, 11, 407; doi:10.3390/mi11040407 www.mdpi.com/journal/micromachines Micromachines 2020, 11, x 2 of 25 complex evolvement caused by nanoindentation at low temperatures can be observed intuitively [15– Micromachines 2020, 11, 407 2 of 25 18]. Low temperature nanoindentation has developed in nearly the past three decades. However, the investigationsLow temperature on such nanoindentation field are not hasas much developed as high innearly temperature the past nanoindentation three decades. However, [19–23] and the relevantinvestigations commercial on such system field are was not asrelatively much as highrare. temperatureCompared nanoindentationwith various and [19 flexible–23] and ways relevant of applicationcommercial of system in a high was temperature relatively rare. environment, Compared including with various resistance and flexible and laser ways heating, of application basically of allin athe high cooling temperature sources environment,in low temperature including nanoindentation resistance and system laser heating, are cryogenic basically liquids, all the such cooling as liquidsources nitrogen in low temperature(LN2) and liquid nanoindentation helium (LHe) system[24–27]. are Academic cryogenic designers liquids, are such always as liquid dedicated nitrogen to solving(LN2) and the liquiddifficulties helium in applying (LHe) [24 a –low27]. temper Academicature designersenvironment are on always a nanoindentation dedicated to system solving and the retainingdifficulties the in high applying sensitivity a low temperatureand accuracy environment of nanoindentation on a nanoindentation technique. system and retaining the highIn sensitivity this article, and the accuracy methods of and nanoindentation testing theories technique. of indentation at ambient and low temperature, includingIn this micro-hardness article, the methods testing and and testing nanoindentation theories of indentation testing, are at introduced. ambient and Several low temperature, stages of nanoindentationincluding micro-hardness systems capable testing of and testing nanoindentation at low temperatures testing, are discussed introduced. in detail. Several The stages major of designnanoindentation elements systemsfeatured capable in the ofsystems testing atare low de temperaturesscribed in relation are discussed to their in low detail. temperature The major functionality.design elements Influence featured factors in the systemsleading areto describedmeasurement in relation error, toincluding their low contact temperature thermal functionality. drift and variationInfluence of factors testing leading system to measurementitself under a error,low temp includingerature contact environment, thermal driftare also and presented. variation of Current testing applicationsystem itself status under of a lowlow temperature temperature environment, indentation aretechnique also presented. is introduced Current in application testing materials status of respects:low temperature metallic indentation materials, techniquesemiconductor is introduced materials, in testingand ceramic materials materials. respects: A metallicsummary materials, of the developmentsemiconductor on materials, low temperature and ceramic nanoindentation materials. A summarytechniques of and the developmentperspectives of on the low technique temperature are concluded.nanoindentation techniques and perspectives of the technique are concluded. 2. Methods Methods of of Indentation Indentation Ever since people found found the the mechanical mechanical properties properties of of material material can can be be investigated investigated artificially, artificially, differentdifferent kinds kinds of of testing testing methods methods have have been been develo developedped through through destroying destroying the the original original structure structure of theof thespecimen. specimen. An impression An impression can be can obtained be obtained on the onsurface the surface of one material of one material permanently permanently by another by sharpanother object sharp through object through a certain a contacting certain contacting load. The load. size The of sizethe impression of the impression was logically was logically related related with thewith “hardness” the “hardness” of the of theimpressed impressed material, material, which which became became the the origin origin of of the the modern modern indentation technique.technique. InIn thisthis section, section, we we will will introduce introduce working working principles principles of two diofff erenttwo indentationdifferent indentation techniques, techniques,micro-hardness micro-hardness and nanoindentation, and nanoindentation, which are widely which applied are widely in academic applied research, in academic and analysis research, of andthe twoanalysis techniques, of the two respectively, techniques, will respectively, be discussed. will be discussed. 2.1. Micro-Hardness Micro-Hardness Testing Testing A representative system of of micro-hardness micro-hardness test test is is shown shown in in Figure Figure 11a,a, containing electric motor, loadload sensor,sensor, indenter,indenter, and and optical optical microscope. microscope. During During an indentationan indentation process, process, the electric the electric motor motor drives drivesthe indenter the indenter moving moving down alongdown zalong axis z until axis the until reading the reading of the of load the sensor load sensor reaches reaches target target value. value.After a After few secondsa few seconds containing containing a target a target load (within load (w 10ithin s),the 10 s), indenter the indenter rises up rises from upthe from surface the surface of the ofspecimen. the specimen. Then, theThen, optical the microscopeoptical microscope moves along move thes along x axis tothe replace x axis theto positionreplace the of indenter position and of indenterenables researchersand enables to researchers observe the to impression observe the caused impression by indenter caused through by indenter a charge through coupled a charge device coupled(CCD) camera. device (CCD) camera. Figure
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