FR3075983A1 - Nano-manipulation device and characterization method using such a device - Google Patents

Nano-manipulation device and characterization method using such a device Download PDF

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FR3075983A1
FR3075983A1 FR1762934A FR1762934A FR3075983A1 FR 3075983 A1 FR3075983 A1 FR 3075983A1 FR 1762934 A FR1762934 A FR 1762934A FR 1762934 A FR1762934 A FR 1762934A FR 3075983 A1 FR3075983 A1 FR 3075983A1
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nano
sample
device
rotary plate
preceding
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Jean-Louis Mansot
Yves Bercion
Andi Mikosch Cuka
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Des Antilles, University of
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Des Antilles, University of
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Priority to FR1762934A priority patent/FR3075983A1/en
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    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/02Details
    • H01J37/20Means for supporting or positioning the objects or the material; Means for adjusting diaphragms or lenses associated with the support
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS, OR APPARATUS
    • G02B21/00Microscopes
    • G02B21/24Base structure
    • G02B21/26Stages; Adjusting means therefor
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS, OR APPARATUS
    • G02B21/00Microscopes
    • G02B21/32Micromanipulators structurally combined with microscopes
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/20Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
    • H01J2237/206Modifying objects while observing
    • H01J2237/2062Mechanical constraints
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/20Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
    • H01J2237/206Modifying objects while observing
    • H01J2237/2067Surface alteration
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/20Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
    • H01J2237/208Elements or methods for movement independent of sample stage for influencing or moving or contacting or transferring the sample or parts thereof, e.g. prober needles or transfer needles in FIB/SEM systems
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/26Electron or ion microscopes
    • H01J2237/28Scanning microscopes
    • H01J2237/2813Scanning microscopes characterised by the application

Abstract

The invention relates to a nano-manipulation device comprising two arms capable of moving in the three directions of space with nanometer positioning accuracy. Each of these two arms further comprises a lateral rotary plate configured to hold and rotate a sample holder, said sample holder being configured to receive at least one nano-tool. The invention also relates to a method of characterization using such a nano-manipulation device.

Description

FIELD OF THE INVENTION

The present invention relates to the field of nano-manipulation. The invention relates more particularly to a nano-manipulation device. It will find, for advantageous but non-limiting applications, nanosampling of samples, mechanical or physical characterization of nanosamples, and the study of friction phenomena on a nanometric scale.

TECHNOLOGICAL BACKGROUND

Friction and wear are phenomena inherent in any mechanical system comprising two bodies in contact and animated by relative movements. These phenomena appear in the most elementary systems (micromechanics) to the most complex (internal combustion machines, gearboxes, braking systems, joints, prostheses, etc.).

Friction is defined as the force that opposes the relative sliding of two bodies in contact. This phenomenon generates a loss of energy, reducing the efficiency or the yield of the mechanical systems, and, when it becomes important, it is accompanied by a release of heat at the level of the contact and damage (wear) of the surface of the friction parts. This damage is one of the major causes of damage to mechanical systems, resulting in high maintenance costs, and a reduction in the life of the equipment.

It is thus estimated, for industrialized countries, that the energy losses generated by friction represent between 1.5 to 3% of their gross national product (GNP). Associated wear represents 30% of the causes of damage in mechanical applications. It is clear that better control of friction and wear phenomena would allow significant energy savings associated with increasing the efficiency of mechanical equipment, reducing maintenance operations and increasing their service life. , effectively contributing to a reduction in negative impacts on the environment by significantly reducing energy costs and therefore the associated greenhouse gas emissions.

The currently known means for combating friction and wear of mechanical parts is lubrication which consists in introducing, between the friction surfaces, a solid, gel, liquid or gaseous material which facilitates the sliding of said surfaces (reduction of friction) and forms a protective film on the contacting surfaces (wear reduction).

The development of lubricants and their evaluation result from an understanding of their operating mode resulting from basic and applied research. This understanding requires the development of assessment tests using scientific instruments, called tribometers.

These tribometers are used to study the phenomena of friction between two surfaces in contact.

More particularly, a tribometer makes it possible to generate in a controlled manner a relative movement between two surfaces in contact and to quantify the phenomena of friction between these two surfaces in contact.

These tribometers ultimately make it possible to qualify lubricants formulated under real conditions of use.

Many tribometers have thus been developed on a macroscopic scale. For example, alternating or rotary ball / plane tribometers can be used for studying limit lubrication regimes, roller or roller / plane tribometers can be used for studying mixed and elastohydrodynamic lubrication regimes, the tribometer four balls can be used for extreme pressure testing. These instrumented tribometers make it possible to measure, on samples from millimeter to centimeter (macroscopic scale), the coefficient of friction, wear, electrical contact resistance. By carrying out additional analyzes by different characterization techniques, such as electron microscopy for example, it is then possible to characterize the worn surfaces, to know the composition of the wear debris and films formed on the surfaces during friction.

However, these known tribometers, allowing macro-manipulation of parts to generate their relative friction, are not suitable for the study of physical and / or chemical phenomena occurring at the level of contact during friction. To study these phenomena, it is indeed necessary to generate and quantify them on the nanometric scale. The study of physical and / or chemical phenomena occurring at the level of contact between parts during their relative friction therefore requires a tribometer adapted to the controlled generation of relative nano-movements of nanometric parts and to the characterization of these relative movements.

Indeed, the researches developed in tribology during the last fifty years have clearly demonstrated the importance of the processes occurring at the atomic or molecular scale (nanometric scale) in the sliding interface, ie in the space contained in the contact between surfaces. This research has proven the need to study these phenomena to further develop new additives that reduce friction and wear. This need is all the more imperative since the current industrial context tends to replace conventional metallurgy (ferrous alloy) and to harden operating conditions to increase the efficiency of thermal machines.

In order to meet this need, it is currently known to use atomic force microscopes (AFM), which exploit the contact between the end of a nanometric tip and a surface of a sample to visualize the topography of the surface. . The diverted use of AFM as tribometers allows the measurement of nanometric properties of the sample, but does not allow the visualization of the sliding interface between the tip and the surface and therefore does not allow the study in real time of the processes physicochemicals occurring in situ in contact. The diverted use of AFMs as tribometers is also essentially limited to a geometrical configuration tip / plane, and does not allow to consider other geometric configurations of contact. Furthermore, the AFM is not compatible with complementary characterization techniques in real time, in particular for direct visualization of the contact during friction by electron microscopy.

To overcome this limitation, document WO 2011137451 A2 discloses the construction of an AFM on a sample of transmission electron microscopy sample. Such a device has for example made it possible to study in real time the sliding behavior at the nanometric scale of nanoparticles of solid lubricants such as carbon onions, carbon blacks, and the fullerenes of WS2 and MoS2. However, the quantification of the forces applied to the contact (normal force and tangential force) remains difficult, which limits the knowledge that can be obtained from the coefficient of friction. In addition, three other important limitations affect this device: - the preparation of the sample consists of depositing particles on an AFM support, which makes it a poorly controlled, even random and hazardous preparation, - it is impossible to work under different atmospheres or in a liquid medium, because, in transmission electron microscopy, a secondary vacuum or an ultra-vacuum is generally required, and - it is necessary to use other equipment to obtain certain mechanical characterizations, such as mechanical characterizations in traction, in compression for example.

An object of the present invention is to at least partially overcome the drawbacks of the abovementioned tribometers.

In particular, an object of the present invention is to propose a nano-manipulation device allowing at least one of: - the controlled preparation, on the nanometric scale, of a nanometric sample to be characterized, - the controlled generation, on the nanometric scale, of friction over nanometric distances on the surface of the sample, and this, preferably, for a plurality of geometric contact configurations, - a precise quantification of the forces applied to the contact, - the work under different atmospheres, even in a liquid medium, and - mechanical characterizations, in particular in tension and compression.

Preferably, the device according to the invention also aims to at least partially overcome the drawbacks of a tribometer obtained by construction of an AFM on a support of transmission electron microscopy sample and allowing direct visualization of the nanometric contact at during friction.

SUMMARY OF THE INVENTION

A first aspect of the invention relates to a nanomanipulation device, intended to equip a microscope stage.

Advantageously, the device comprises: - a base, - a first arm and a second arm secured to the base by their respective proximal end, each of said first and second arms being configured so that their respective distal end moves in three directions of space different from each other, preferably with a positioning accuracy of less than or equal to 1 nanometer, - a first lateral rotary plate fixed to the distal end of the first arm and configured to be rotated, preferably with a positioning accuracy of less than 0.01 degree, - a second lateral rotary plate fixed to the distal end of the second arm, and configured to be rotated, preferably with a positioning accuracy of less than 0.01 degree, - at least one tool holder fixed, preferably removably, to at least one of the first and second plates r lateral otatives, preferably with a positioning accuracy of less than 0.01 degrees, and - a central rotary plate fixed on the base in a middle position between the first and second arms, configured to support, preferably removably, and put in rotation a sample holder, preferably with a positioning accuracy of less than 0.01 degrees.

The device according to the first aspect of the invention thus has, for each of the distal ends of the first and second arms, three degrees of freedom in translation and a degree of freedom in rotation. To these eight degrees of freedom is added a ninth degree of freedom in rotation coming from the central rotary plate. It therefore has a total of nine degrees of freedom, allowing various relative movements and positions between the first arm, the second arm, the first lateral rotary stage, the second lateral rotary stage and the central rotary stage.

The device is further configured to perform these movements with nanometric positioning precision.

The movements achievable by the device according to the first aspect of the invention according to the nine degrees of freedom make it possible to manipulate a sample. In particular, one objective of this manipulation is to establish contact with the sample, on a nanometric scale.

The device according to the first aspect of the invention thus allows at least one of: - the controlled preparation, on the nanometric scale, of a nanometric sample to be characterized, - the controlled generation, on the nanometric scale, of 'friction over nanometric distances to the surface of the sample, preferably for a plurality of geometric contact configurations, and precise quantification of the forces applied to the contact. Advantageously, the at least one tool holder is configured to receive, preferably removably, at least one nano-tool taken from: a nano-sample holder, a nano-tip, a nano-clamp, a nano- pipette, a nano-hook, a nano-scalpel and a nano-force sensor for example. This list is not exhaustive, however.

Such a nano-tool can be dedicated to the manipulation at the nanometric scale of a sample. Each nano-tool preferably has at least one nanometric dimension at one of its ends.

Advantageously, the nanotool is driven via the tool holder fixed on the lateral rotary plate of the corresponding arm, by a combination of movements of said arm and said lateral rotary plate.

The device thus makes it possible to establish direct contact between the nanotool carried by the tool holder and the sample to be characterized. It allows in particular the extraction of nano-fragments or nanoparticles from a sample of micrometric to millimeter dimensions, the nano-manipulation of these nanofragments or these nanoparticles, the nano-cutting and the nano-machining of the sample, the controlled deposition and / or fixing of the nano-fragments or nanoparticles on the nano-supports and / or nano-tools and the performance of mechanical characterizations at the nanometric scale of the nano-fragments or nanoparticles of the sample, in particular in tension, bending and compression.

More particularly, a displacement of the arm and / or of the lateral rotary plate carrying the nanotool and / or of the central rotary plate makes it possible for example to generate in a controlled manner friction at the level of the contact between the nanotool and the sample, at the nanoscale.

Furthermore, the use of different nano-tools for the first and second arms can make it possible to take at least one part of the sample so as to establish contact between said part of the sample, taken for example by a first nano- tool, and a second nano-tool. As before, a relative displacement of the first and second arms provided with their respective lateral rotary plates makes it possible to generate friction at the level of said contact, on the nanometric scale.

Such a manipulation device with nine degrees of freedom therefore has a modularity making it possible to achieve a plurality of geometric configurations for contact with a sample, on a nanometric scale, and to exert at least one force, for example friction, at the level of this contact.

According to an advantageous possibility, this device has a space requirement and an operation compatible with a scanning electron microscopy chamber, so as to be able to visualize the physical and / or chemical phenomena occurring within the contact during friction, at scale. nanoscale.

A second aspect of the invention relates to a tribological characterization system at the nanometric scale comprising a microscope, preferably a scanning electron microscope, for example an environmental scanning microscope, and a nano-manipulation device as introduced above, the device equipping a microscope stage. It is therefore possible to characterize a sample on a nanometric scale under different atmospheres, even in a liquid medium.

A third aspect of the invention relates to a tribological characterization process at the nanometric scale implementing said tribological characterization system at the nanometric scale

Advantageously, this method comprises the following stages: - depositing a sample, preferably in nanometric form, on the removable sample holder fixed to the central rotary stage, - fixing at least one nanotool on the at least one holder tool from at least one of the first and second lateral rotary plates, - Visualize by microscopy the sample deposited on the removable sample holder, - Establish contact between the at least one nanotool and the sample, - Apply at least one force at the level of the contact by actuating at least one of the first arm, the second arm, the first lateral rotary stage, the second lateral rotary stage and the central rotary stage, - Visualize the contact, so to observe and / or measure at least one physico-chemical phenomenon at the contact level when applying the at least one force.

The method according to the invention thus makes it possible to carry out a tribology experiment at the nanometric scale, for example by generating friction at the level of the contact, and to visualize the contact during friction, so as to observe and / or measure in real-time physical and / or chemical phenomena occurring within the contact during friction, on the nanometric scale.

Another aspect of the invention relates to a kit comprising a base, a first arm, a second arm, a first lateral rotary plate, a second lateral rotary plate, at least one tool holder and a central rotary plate intended to be assembled for forming the nanomanipulation device according to the first aspect of the invention.

BRIEF INTRODUCTION OF THE FIGURES Other characteristics, objects and advantages of the present invention will appear on reading the detailed description which follows, and with reference to the appended drawings given by way of nonlimiting examples and in which: - Figure 1 shows a cross-sectional view of the nanomanipulation device according to a first embodiment of the invention; - Figure 2 shows a perspective view of the nanomanipulation device according to a second embodiment of the invention; - Figure 3 shows a perspective view of the nanomanipulation device according to a third embodiment of the invention; - Figures 4A and 4B illustrate a tribology experiment at the nanometric scale carried out using the nano-manipulation device according to an embodiment of the invention. FIG. 4A is an image of scanning electron microscopy in secondary electrons. Figure 4B is a dark field transmission scanning electron microscopy image; - Figures 5A to 5M show different tool holders and nano-tools usable by the nanoscale manipulation device according to the invention. FIGS. 5A to 5C illustrate different tool holders equipped with different nano-tools. Figures 5D to 5M illustrate different nano-tools; - Figure 6 is a diagram of the tribological characterization process at the nanometric scale according to an embodiment of the invention.

The drawings are given as examples and are not limitative of the invention. They constitute schematic representations of principle intended to facilitate the understanding of the invention and are not necessarily on the scale of practical applications.

DETAILED DESCRIPTION The invention according to its first aspect comprises in particular the following optional characteristics which can be used in combination or alternatively: - The at least one tool holder is configured to receive, preferably removably, at least one nano- tool taken from: a nano-sample holder, a nano-tip, a nano-hook, a nano-scalpel, a nano-clamp, a nano-pipette and a nano-force sensor. - The device further includes the sample holder removably attached to the central rotating stage. - At least one of the first and second arms, the first and second lateral rotary plates and the central rotary plate comprises an inertial piezoelectric actuator allowing first movements, called large amplitudes, at first speeds, called high, and second movements, called small amplitudes, at second speeds, said to be low, so as to allow a great latitude of positioning with a great precision of positioning. - The first and second arms, the first and second lateral rotary plates and the central rotary plate are configured to operate at a pressure higher than atmospheric pressure and in a pressure range extending from atmospheric pressure to a pressure of 10 ' 5 Pa, and preferably in a pressure range extending from atmospheric pressure to a pressure of 10'9 Pa. - The device is configured to equip an electronic scanning microscope stage, for example environmental, the device having preferably overall dimensions less than 13.5 cm in length, 6 cm in height and 4 cm in width. - At least one of the base, the first and second arms, the first and second lateral rotary plates and the central rotary plate is made of a non-magnetic material. - The device is non-magnetic. - The sample holder is made of a non-magnetic material. - At least one of the first and second lateral rotary plates is electrically and / or thermally isolated from the at least one tool holder. - The device further comprises interference displacement sensors configured to measure displacements of the first and second arms along three orthogonal axes x, y and z. - The device comprises at least two tool holders each configured to receive, preferably removably, a nanotool and jointly configured so that the end of each of the two nanotools can be placed in the eucentric position. - The device further comprises at least one force sensor configured to measure a force applied and / or received at the level of at least one of the first and second arms, the at least one tool holder and at least one nano -tool. - The device further comprises a circuit for applying and measuring voltage and current configured for the acquisition of current voltage characteristics of a sample or of a contact between a sample and at least one nanotool configured to be received by at least one tool holder. - The device further comprises at least one of: a cooling system, for example a Peltier effect cell, and a heating system, for example a Joule effect cell. The invention according to its third aspect notably comprises the following optional characteristics which can be used in combination or alternatively: - The fixing of the at least one nanotool comprises a first fixation of a first nanotool on a first door tool fixed to the first lateral rotary plate, and a second fixing of a second nanotool on a second tool holder fixed to the second lateral rotary plate, said method further comprising taking a part of the sample with one of the first and second nanotools, actuating at least one of the first arm, the second arm, the first lateral rotary stage, the second lateral rotary stage and the central rotary stage, so as to fix said part of the sample on one of the first and second nano-tools, - Establishing contact between the at least one nano-tool and the sample includes establishing contact between the sample portion attached to one of the first and second nano-tools, and the other of the first and second nano-tools. - The method further comprises the following step, after sampling: - Remove the removable sample holder so as to allow insertion of at least one detector, for example a detector of transmitted electrons, between the central rotary stage and the first and second nanotools. - The method further comprises, after the application of the at least one force at the contact level, at least one measurement taken from a measurement of said force, a measurement of a reaction force and a measurement of a displacement relative of the at least one nanotool. - The method further comprises a calibration of the at least one nanotool so as to determine, for example, an elastic constant of said at least one nanotool.

In the present patent application, the directions of space are defined according to an orthonormal coordinate system xyz illustrated in FIGS. 1 to 3. The expression "horizontal" means an orientation in the direction x or y, and by "vertical", a orientation in z direction. In the following, the length is taken along y, the height is taken along z and the width is taken along x.

In the context of the present invention, the term “nanometric scale” means a scale having at least one dimension less than a few hundred nanometers, and preferably less than a few tens of nanometers. Such a scale is used to represent extremely small structures that can be found at the molecular level.

The terms preceded by a prefix "nano-", such as "nanomanipulation", "nano-tools", "nano-needles", "nano-clamp" for example, mean that these terms concern an action or a system that can be represented on a nanometric scale.

In the following, the description is based on the terminology "nano-". This terminology is not however exclusive of the invention, and can be replaced by the terminology "micro-", meaning in a similar way that the terms preceded by a prefix "micro-" relate to an action or a representable system on a micrometric scale.

The relative movement of two bodies which touch each other can be considered, at any point on their contact surface, as the combination of three elementary movements defined according to the usual methods of kinematics: these elementary movements are sliding, pivoting and rolling .

Rolling and pivoting can only occur if one of the bodies is rotated. On the other hand, a rotation will not necessarily lead to the existence of a rolling and pivoting movement at the level of the contact surfaces.

In the theoretical framework of tribology, each of these three movements can be, independently of the other two, prevented by adhesion, or as the case may be, slowed down by friction.

Friction is defined as the force that opposes the relative sliding of the two bodies.

Friction can generate a sliding interface at the contact. This sliding interface includes physical and / or chemical phenomena occurring “within” the contact.

The nano-manipulation device according to the first aspect of the present invention finds in particular for application the generation and study of friction phenomena on the nanometric scale, that is to say at the level of a contact between two body having at least one nanometric dimension, and more particularly within this contact. The invention is described in detail in the following, with reference to the attached figures.

The nano-manipulation device 1 according to the first aspect of the invention is in particular intended to carry out manipulations and / or experiments on a sample. This sample can in particular be hard material, soft material, organic or inorganic, in microscopic form.

With reference to FIGS. 1, 2 and 3, a preferred embodiment of this device 1 comprises a first arm 11 opposite a second arm 12 each mounted on the same support 6. The proximal ends of these first and second arms 11, 12 can be spaced a distance of between 6 cm and 12 cm, and preferably of the order of 10 cm.

A central rotary plate 7, the axis of rotation of which is oriented in the direction z, is fixed on the support 6 between the first and second arms 11, 12, in a so-called central position, preferably equidistant from the proximal ends of the first and second arms 11, 12.

This central rotary plate 7 is preferably configured to receive and rotate a removable sample holder 8.

Each of the first and second arms 11, 12 is configured to move in the three directions of space x, y and z.

A design of these first and second arms 11, 12 can advantageously be identical. The design of the first arm 11 described below can therefore be adapted mutatis mutandis to the design of the second arm 12.

The first arm 11 comprises a motorized translation plate 1x along x, a motorized translation plate 1y according to y and a motorized translation plate 1z according to z. These 1x, 1y, 1z unidirectional translation plates are assembled for example by means of two assembly elements 2, so that the displacement in translation of one of the 1x, 1y, 1z plates is perpendicular to the displacement of the two others.

The first arm 11 thus has a distal end free to move in all directions of space, by combining the displacements of each of the plates 1x, 1y, 1z of unidirectional translation.

A first lateral rotary plate 31 is fixed at the free end of the first arm 11, for example on the plate 1z of translation along z. The axis of rotation of this first lateral rotary plate 31 can advantageously be oriented in the direction y. This first lateral rotary plate 31 is preferably configured to perform rotations on an angular sector of 180 °. A bisector, called the middle position, of this angular sector is preferably parallel to the direction z. The first lateral rotary plate 31 thus makes it possible to perform ± 90 ° angle rotations from said median position.

The 1x, 1y, 1z unidirectional translation stages are advantageously configured to allow both large and small amplitude translational movements.

The translational displacements of each of these 1x, 1y, 1z plates are made for example by inertial piezoelectric motors, allowing large amplitude displacements, of the order of a few millimeters, at high speeds, of the order of a few tens of pm / s to a few mm / s, with a positioning accuracy of between 1 pm and 10 pm, and small amplitude displacements, from a few nanometers to 1 pm, at speeds from a few nm / s to a few tens of nm / s with a positioning accuracy of the order of or less than a nanometer.

The first lateral rotary plate 31 and the central rotary plate 7 are advantageously configured to allow both large and small amplitude rotational movements.

These rotational displacements can be achieved by inertial piezoelectric motors, as for translational displacements, in particular allowing large amplitude rotations at high speeds, of the order of ten degrees / s, with positioning accuracy of the order of the degree, and small amplitude rotations, of the order of 0.1 ° to 0.01 °, with high positioning accuracy, of the order of 0.001 °.

The various plates 1x, 1 y, 1 z, 7, 31 are preferably equipped with displacement sensors. These displacement sensors can for example be miniature interference sensors, of the Michelson type, configured to measure a displacement with a measurement accuracy of less than a nanometer.

Preferably, the device 1 comprising the base 6, the first and second arms 11, 12, the first and second lateral rotary plates 31, 32 and the central rotary plate 7 is made of non-magnetic materials (316L stainless steel, aluminum, titanium by example). Such a non-magnetic device 1 can thus be used within an electron microscope without disturbing an electron beam display.

As illustrated in FIGS. 1 to 3, a first tool holder 41 is fixed to the first lateral rotary plate 31. This first tool holder 41 may have a free end extending mainly horizontally as in FIG. 2 or inclined, by example of an angle β relative to the horizontal, as in FIG. 1. This first tool holder 41 can advantageously be removable, so as to allow the use of various tool holders.

Different tool holders 41, 42, illustrated in FIGS. 2, 3 and 5A to 5C, can thus be fixed on the first lateral rotary plate 31 at the free distal end of the first arm 11.

Such tool holders 41, 42 can be for example: - an inclined tool holder having an angle β of between 45 ° and 90 ° and preferably between 65 ° and 80 ° (FIG. 1 and 5C), - a tool holder horizontal (Figure 2 and 5B), - a tool holder with double angle return (Figure 3 and 5A), used alone or in addition to a horizontal tool holder for example, having right angles ai, 2 = 90 ° or between 45 ° and 160 ° for example. Other configurations of these tool holders 41, 42 can be envisaged, depending on a specific need or a particular application. The tool holders 41, 42 are preferably non-magnetic.

The tool holders 41, 42, for example the first tool holder 41, are configured to receive and fix at least one nanotool 51, 52, for example a first nanotool 51.

This first nano-tool 51 may for example be a tip or a needle, called a nano-tip or a nano-needle, having nanometric dimensions at one end, for example a radius of curvature between 50 nm and 300 nm.

Other nano-tools 51, 52 are partially illustrated in Figures 4 and 5D to 5M

Such nano-tools 51, 52 can be for example: - a nano-needle (FIG. 5D), - an angled nano-needle, having an angle including between 90 ° and 170 ° for example (FIG. 5E), - a nano-needle provided with a nano-sphere at its end (Figure 5F), - a support nano-blade (Figure 5G) - a nano-lasso (Figure 5H) - a nano-hook (Figure 5I) - a nano- pipette (Figure 5J) - a nano-scalpel (Figure 5K and 5L) - a nano-clamp (Figure 5M) Other configurations of these nano-tools 51, 52 can be envisaged, depending on a specific need or d 'a particular application. The nano-tools 51, 52 can in particular be instrumented, and include for example at least one force sensor. They can, for example, allow a measurement of electrical and / or thermal conductivity at the level of a sample or of a contact between the sample and one end of said nano-tools 51, 52.

The nano-tools 51, 52 can therefore be made of a thermal and / or electrical conductive material. Alternatively, they can be made of an insulating material, for example glass. They can be functionalized by surface treatment or by depositing a thin layer on the surface of said nano-tools 51, 52. This thin layer can for example be insulating or thermally and / or electrically conductive, mineral or organic, chemically reactive or inert .

Given their small dimensions and their low mass, the nano-tools 51, 52 can be partially or totally made of magnetic materials (ferromagnetic or paramagnetic for example), without this significantly altering an observation under an electron beam during their use in a scanning electron microscope (SEM) in particular.

Different manufacturing techniques can make it possible to manufacture these nano-tools 51, 52, such as EDM, ion abrasion, electrolysis or a fusion-stretching technique for example.

The tool holders 41, 42 and nano-tools 51, 52 can in particular be chosen according to a type of manipulation and / or of experience to be carried out via the device 1 of nano-manipulation. They can be used for the purposes of sample collection, sample preparation or shaping, physical and / or tribological characterization.

The device 1 is thus advantageously modular and versatile.

The nano-manipulation device 1 makes it possible in particular to establish contact between one end of a nano-tool carried by one of the first and second arms 11, 12 and a sample, said sample being carried by the support d sample 8 or fixed to the other among the first and second arms 11, 12.

The sample holder 8 can be functionalized as required, for example by adding complementary supports 9 adapted to the manipulations and / or the experiments to be carried out.

The first and second arms 11, 12 also make it possible to exert at least one force at the level of contact with the sample, by combination of displacements in translation and / or in rotation of the various plates. This force applied to the contact on the nanometric scale can be of the order of a few nano-Newtons to a few micro-Newtons.

Such a force, for example normal or tangential to the surface of the sample, can cause friction and / or deformation on the surface of the sample.

Advantageously, instrumentation of the nano-tools 51, 52 by means of force sensors for example, makes it possible to measure said force or a reaction force of the sample so as to characterize the sample mechanically.

The experiments achievable by means of the device 1 can therefore be traction and / or compression and / or indentation tests, normal and / or lateral force measurements applied to the nano-contact. These experiments can in particular make it possible to determine a coefficient of friction and / or a Young's modulus and / or a hardness of the sample.

The device 1 makes it possible in particular to carry out tribology experiments according to different contact configurations. According to different combinations of tool holders 41, 42 and nano-tools 51, 52 fixed on the first and second arms 11, 12, the contact can be made in tip / plane or ball / plane configuration for example (FIG. 2), or in tip / cylinder configuration or crossed cylinders for example (Figure 3).

The device 1 provided with at least one nano-scalpel allows for example nano-machining or the production of nano-cuts of samples.

As part of manipulations or experiments requiring temperature control, preferably in a temperature range between -10 ° C and + 200 ° C, different cooling or heating systems can be coupled to device 1.

For example, for handling at temperatures below room temperature, a Pelletier type cooling system (not shown) can be coupled to the tool holders 41,42.

For handling at temperatures above ambient temperature, a heating system by Joule effect or by lamp (not shown) can be coupled to the tool holders 41, 42. Such a heating system by lamp, equipped for example with a converging lens allowing a focusing of light on an area comprising the sample, can advantageously be moved outside the field of observation of said sample.

The first and second lateral rotary plates 31, 32 are preferably thermally and / or electrically insulated from the tool holders 41, 42, for example by a Teflon or machinable ceramic insulation piece.

The device 1 can be supplied with electrical energy and controlled by hardware and software means known to those skilled in the art. The device 1 can thus be equipped with wired connections and / or connectors provided for supplying electrical energy and controlling said device 1. Optionally, a battery, for example on board, can provide this supply.

The device 1 is preferably configured to receive and execute control commands, and to collect and transmit measurements.

The nano-manipulation device 1 is in particular configured to be compatible with observation of the sample by scanning electron microscopy. The device 1 can in particular be used in a conventional scanning electron microscope, in an environmental scanning electron microscope or in a microscope with a double beam of ions and electrons (often called FIB-SEM Dual Beam or simply Dual Beam, d 'after the English "Focused Ion Beam - Scanning Electron Microscope Dual Beam").

The device 1 equipping such a microscope advantageously forms the tribological characterization system on the nanometric scale according to the second aspect of the invention. This system can also include a dedicated connector allowing on the one hand to supply and control the device 1 within a SEM chamber and on the other hand to collect and transmit the measurements.

The device 1 advantageously has a limited size, preferably less than 4 X 13.5 X 6 cm according to a width, a length and a height respectively, so as to be compatible with the dimensions of a small SEM observation chamber. (typically with a diameter of 250 mm) and / or a SEM airlock. Such dimensions in width, length and height also make it possible to limit any mechanical drift resulting from thermal expansions.

Furthermore, the device 1 is configured so that the nano-tools 51, 52 and / or the sample holder 8 can be positioned in line with a pole piece 20 of objective lens of a SEM, at a distance vertical working range between 2 mm and 30 mm, preferably 10 mm, without disturbing the operation of the electronic column of the SEM.

In particular, a relative arrangement of the various elements constituting the device 1 (in particular the central rotary plate 7 and the first and second arms 11, 12 provided with their respective lateral rotary plates 31, 32 and tool holders 41, 42 equipped with nano -tools 51, 52) allows observation under an electron beam under normal observation conditions, preferably without interaction with the electronic column.

The tool holders 41, 42 are preferably arranged so that the end or an active part of the nano-tools 51, 52 in contact with the sample to be observed can be positioned in a so-called eucentric position. The eucentric position is at the intersection between the axis of the electron beam (generally along z) and an axis of rotation (for example along y) around which the observed sample can be rotated without modification of the position (x, y, z) of the part of the sample observed during the rotation.

The device 1 advantageously makes it possible to orient the first and second arms 11, 12 so that a sliding interface at the contact between a nanotool 51, 52 and a sample is parallel to the incident electron beam of the SEM. It is thus possible to visualize the sliding interface by scanning electron microscopy in STEM transmission (from English "Scanning Transmission Electron Microscopy").

The various elements constituting the device 1 are preferably made of non-magnetic material, such as aluminum or an aluminum alloy and titanium for example.

The various elements constituting the device 1 are preferably compatible with vacuum operation. The device 1 is in particular configured to operate at pressures between atmospheric pressure and 10 "5 Pa (a pressure of 10" 5 Pa corresponding to a high vacuum), and preferably at pressures between atmospheric pressure and 10 "9 Pa (a pressure of 10" 9 Pa corresponding to the ultra-vacuum). The device 1 can thus be used for various applications ranging from experiments on organic soft matter or liquids to experiments in ultra-vacuum or experiments under partial pressures of very pure gases or in mixture.

Advantageously, the sample holder 8 fixed on the central rotary plate 7 is removable and can be removed so as to be able to insert a detector 21, for example a STEM-BF / DF or HAADF detector (from English “Scanning Transmission Electron Microscopy-Bright Field / Dark Field or High Angle Annular Dark Field ”) for transmission observations of a sample fixed on a nanotool. Such observations in STEM configuration indeed require placing the sample to be observed between a pole piece 20 and the STEM detector 21, along the electron beam, as illustrated in FIGS. 2 and 3.

The device 1 advantageously makes it possible to orient the first and second arms 11, 12 so that a sliding interface at the contact between a nanotool and a sample is parallel to the incident electron beam of the SEM in STEM configuration.

The STEM detector 21 can thus collect electrons transmitted through the sample and in particular through the contact established between the sample and the end of the nano-tool, for example a nano-needle 51, to form for example a dark field image as shown in Figure 4B. In this FIG. 4B, and in the corresponding FIG. 4A acquired by secondary electron imaging, the nano-needle 51 has a spherical end in contact with the surface of a carbon nano-disc fixed on a nanosupport 52.

This visualization of the nanodisc advantageously makes it possible to precisely position the point on a part of the surface of the nanodisc free of undesirable particles for the measurement.

The device 1 placed in a SEM thus makes it possible to image physical and / or chemical phenomena occurring at the nanometric scale within the contact and / or the sample, in real time during the experiment.

The device 1 can advantageously be used in combination with different imaging techniques, such as secondary electron imaging (Figure 4A), backscattered electron imaging, transmitted electron imaging (Figure 4B), imaging by X or X-EDS photons (from the English “X-ray Energy Dispersive Spectroscopy”), in particular within a SEM. The device 1 can also be used under a standard or confocal photonic microscope, under a Raman and / or infrared spectrometer microscope, and under a fluorescence and / or photoluminescence spectrometer microscope for example.

Furthermore, a calibration of the device 1 and in particular of the nano-tools 51, 52 can be carried out by measuring a displacement or a deformation of one end of said nano-tools 51, 52, directly on an image for example or via a force sensor, as a function of a force exerted or of a movement imposed by the first arm 11 and / or the second arm 12 carrying said nano-tools 51, 52.

A second aspect of the invention relates to a process 100 for tribological characterization at the nanometric scale using the device 1 for nano-manipulation.

With reference to FIG. 6, a preferred embodiment of this method 100 notably comprises a calibration step 109 of at least one nanotool 51, 52, before carrying out the manipulations and / or experiments to be carried out on a sample . For example, for the calibration 109 of the elasticity of a first nano-tool 51 intended to hold a sample, a compression force sensor can be fixed at a free end of the second arm 12, on a holder. possibly dedicated tool. The first nanotool 51 is fixed 110 to the tool holder of the first arm 11. The first nanotool 51 is then brought into contact with the force sensor and, by displacement of one of the first and second arms 11, 12 , the first nanotool 51 is elastically deformed against the force sensor so as to record a diagram of force applied as a function of a measured displacement. An elastic constant of this first nano-tool 51 can then be deduced from this diagram. This calibration 109 can be done after introduction of the nano-manipulation device 1 into the SEM.

After calibration 109, the force sensor is removed and a second nano-tool, such as a micro-clamp, a nano-clamp or a nano-tip, is fixed 110 to a tool holder of the second arm 12, in place of the force sensor. This second nano-tool may have been previously calibrated 109. A few micrograms of the sample to be characterized are deposited 111 on a flat sample support 8 (for example a disc, preferably polished, having a diameter less than or equal to 10 mm and a thickness of between 1 and 5 mm) then placed on the central rotary stage 7. After introduction into the microscope, the sample can be viewed 112 on the sample holder 8 in order to locate a fragment or a part of interest of the sample. The second nanotool 52 then makes it possible, by combinations of translational displacements of the second arm 12 and / or rotational displacements of the central rotary plate 7, to take 114 said part of interest, to manipulate it and to deposit it on the first calibrated nano-tool 51.

The second sampling nano-tool 52 can then be removed in favor of another calibrated nano-tool. The removable sample holder 8 is preferably removed 115 so as to allow insertion of a detector 21 of transmitted electrons (STEM) between the central rotary plate 7 and the nano-tools 51, 52. The device 1 is then reintroduced into the scanning electron microscope. The establishment 113 of a contact between the part of the sample taken from the first nano-tool 51 and the other nano-tool is produced by displacements of the first and second arms 11, 12, and observed in real time by imaging in secondary or backscattered electrons, or by transmission scanning electron microscopy (STEM) after insertion of the 21 STEM detector to the right of the part of interest of the sample.

With the contact established 113 and displayed 117, a normal force can be applied 116 to the contact gradually up to a selected value. This force value can in particular be measured 118 by deformation of the calibrated nano-tools 51, 52.

Slippage is then caused by alternating unidirectional displacement of at least one of the nano-tools 51, 52, advantageously perpendicular to the direction of application of the normal force. This sliding can be an alternating movement, by periodic change of the direction of movement of said nanotool.

The sliding can be controlled by programming, for example movements of at least one of the first and second arms 11, 12, and a sliding speed can be advantageously chosen.

A friction force can therefore be measured 118 in real time by elastic deformation of the nano-tools 51, 52. A friction coefficient can in particular be deduced and an evolution of this friction coefficient can be determined during the experiment, by quantifying the different displacements and / or forces using position and / or force sensors integrated into the translation stages along x, y and z.

Advantageously, an acquisition of images or of a video can be carried out during the experiment, so as to visualize 117 of the phenomena occurring at the level of the contact. This acquisition makes it possible for example to measure displacements and deformations and to verify the measurements possibly acquired by the various position and / or force sensors of the device 1, by post processing of these images.

Another embodiment of the method 100 aims to carry out a tribology experiment for a rotary movement. Only the different steps with respect to the previous embodiment are described below, the other steps being deemed to be identical. The sample to be studied is deposited 111 on a sample support 8 fixed on the central rotary plate 7. This configuration of experiment does not allow visualization 117 of the contact in transmission, the presence of the sample support 8 on the plate central rotary 7 preventing insertion of the detector 21 STEM.

Contact is established 113 between at least one nanotool and an area supporting the sample, without prior sampling. A normal contact load can be applied gradually 116 to a chosen value and the sliding is caused by rotation, continuous or alternating, of the central rotary plate 7. The modifications of the contact zone and of the sample having transited in the sliding interface are followed by imagery (by secondary electrons, backscattered and / or X photoelectrons) at the level of a wear trace, in the immediate vicinity of the contact for example.

The nano-manipulation device 1 and the tribological characterization method 100 make it possible to carry out fundamental experiments to study in particular friction phenomena on the nanometric scale. The results of these experiments can improve an understanding of these friction phenomena, and find applications in the fields of mechanical assembly and lubrication, in order to reduce the deleterious effects due to friction.

The modularity and versatility of the device 1 make it possible to envisage applications in the field of biology for example, such as the characterization of the mechanical properties of capsids, or the characterization of the adhesion forces of microorganisms between them or on a support. Other applications in the pharmaceutical field or in the field of nanotechnologies and nanoelectronics are also possible. The invention is not limited to the embodiments described above but extends to all embodiments falling within the scope of the claims.

Claims (20)

1. Nano-manipulation device (1), intended to equip a microscope stage, characterized in that it comprises: - A base (6), - a first arm (11) and a second arm (12) integral with the base (6) by their respective proximal end, each of said first and second arms (51, 52) being configured so that their respective distal end moves in three directions of space different from each other, preferably with lower positioning accuracy or equal to 1 nanometer, - a first lateral rotary plate (31) fixed to the distal end of the first arm (11) and configured to be rotated, preferably with a positioning accuracy of less than 0.01 degrees, - a second lateral rotary plate (32) fixed to the distal end of the second arm (12), and configured to be rotated, preferably with a positioning accuracy of less than 0.01 degrees, - at least one tool holder (41, 42) fixed, preferably removably, to at least one of the first and second lateral rotary plates (31, 32), preferably with a positioning accuracy of less than 0, 01 degree, and - a central rotary plate (7) fixed on the base (6) in a middle position between the first and second arms (11, 12), configured to support, preferably removably, and to rotate a sample holder (8), preferably with a positioning accuracy of less than 0.01 degrees.
2. Device (1) according to the preceding claim, wherein the at least one tool holder (41, 42) is configured to receive, preferably removably, at least one nano-tool (51, 52) selected from : a nano sample holder, a nano-tip, a nano-hook, a nano-scalpel, a nano-clamp, a nano-pipette and a nano-force sensor.
3. Device (1) according to any one of the preceding claims, in which at least one of the first and second arms (11, 12), the first and second lateral rotary plates (31, 32) and the rotary plate central (7) comprises an inertial piezoelectric actuator allowing first movements, called large amplitudes, at first speeds, called high, and second movements, called small amplitudes, at second speeds, called low, so as to allow a wide positioning latitude with high positioning accuracy.
4. Device (1) according to any one of the preceding claims, in which the first and second arms (11, 12), the first and second lateral rotary plates (31, 32) and the central rotary plate (7) are configured. to operate at a pressure higher than atmospheric pressure and in a pressure range extending from atmospheric pressure to a pressure of 10'5 Pa, and preferably in a pressure range extending from atmospheric pressure to a pressure from 10'6 * * 9 Pa.
5. Device (1) according to any one of the preceding claims, configured to equip an electronic scanning microscope stage, for example environmental, the device (1) preferably having overall dimensions less than or equal to 13.5 cm. in length, 6 cm in height and 4 cm in width.
6. Device (1) according to any one of the preceding claims, in which at least one of the base (6), the first and second arms (11, 12), the first and second lateral rotary plates (31, 32) and the central rotary plate (7) is made of a non-magnetic material.
7. Device (1) according to any one of the preceding claims being non-magnetic.
8. Device (1) according to any one of the preceding claims, in which at least one of the first and second lateral rotary plates (31, 32) is electrically and / or thermally insulated from the at least one carrier. tool (41,42).
9. Device (1) according to any one of the preceding claims, further comprising interference displacement sensors configured to measure displacements of the first and second arms (11, 12) along three orthogonal axes x, y and z.
10. Device (1) according to any one of the preceding claims, comprising at least two tool holders (41, 42) each configured to receive, preferably removably, a nano-tool (51, 52) and jointly configured so that the end of each of the two nano-tools can be placed in the eucentric position.
11. Device (1) according to any one of the preceding claims, further comprising at least one force sensor configured to measure a force applied and / or received at at least one of the first and second arms (11 , 12), the at least one tool holder (41, 42) and at least one nano-tool (51, 52).
12. Device (1) according to any one of the preceding claims, further comprising a circuit for applying and measuring voltage and current configured for the acquisition of current voltage characteristics of a sample or of a contact between a sample and at least one nanotool (51, 52) configured to be received by the at least one tool holder (41,42).
13. Device (1) according to any one of the preceding claims, further comprising at least one of: a cooling system, for example a Peltier cell, and a heating system, for example a cell Joule.
14. Kit comprising a base (6), a first arm (11), a second arm (12), a first lateral rotary plate (31), a second lateral rotary plate (32), at least one tool holder (41 , 42) and a central rotary plate (7) intended to be assembled to form the nano-manipulation device (1) according to any one of the preceding claims.
15. A tribological characterization system at the nanometric scale comprising a microscope, preferably an environmental scanning electron microscope, and a nanomanipulation device (1) according to any one of claims 1 to 13, the device (1) equipping a microscope stage.
16. A method (100) of tribological characterization on the nanometric scale using a tribological characterization system on the nanometric scale according to the preceding claim, comprising the following steps: - depositing (111) a sample, preferably in nanometric form , on the removable sample holder (8) fixed to the central rotary plate (7), - Fix (110) at least one nanos tool (51, 52) on the at least one tool holder (41, 42 ) of at least one of the first and second lateral rotary plates (31, 32), - View (112) by microscopy the sample deposited on the removable sample support, - Establish (113) a contact between the at least one nanotool (51, 52) and the sample, - Apply (116) at least one force at the level of the contact by actuating at least one of the first arm (11), the second arm (12) , the first lateral rotary plate (31), the second rotary plate e lateral (32) and the central rotary plate (7), - Visualize (117) the contact, so as to observe and / or measure at least one physico-chemical phenomenon at the level of the contact during the application (116) of at least one force.
17. Method (100) according to the preceding claim, in which: - the fixing (110) of the at least one nanotool (51, 52) comprises a first fixation of a first nanotool (51) on a first tool holder (41) fixed to the first lateral rotary plate (31), and a second fixing of a second nano-tool (52) on a second tool holder (42) fixed to the second lateral rotary plate (32 ), said method (100) further comprising removing (114) part of the sample with one of the first and second nano-tools (51, 52), by actuating at least one of the first arm (11), the second arm (12), the first lateral rotary stage (31), the second lateral rotary stage (32) and the central rotary stage (7), so as to fix said sample part on one among the first and second nano-tools (51, 52), - The establishment (113) of contact between the at least one nano-tool (51, 52) e t the sample comprises establishing contact between the sample part fixed to one of the first and second nano-tools (51, 52), and the other of the first and second nano-tools (51, 52).
18. Method (100) according to the preceding claim, further comprising the following step, after sampling (114): - Remove (115) the removable sample holder (8) so as to allow insertion of at least a detector (21), for example a detector of transmitted electrons, between the central rotary plate (7) and the first and second nanotools (51, 52).
19. Method (100) according to any one of the three preceding claims, further comprising, after the application (116) of the at least one force at the level of the contact, at least one measurement (118) taken from a measurement of said force, a measurement of a reaction force and a measurement of a relative displacement of the at least one nanotool.
20. Method (100) according to any one of claims 16 to 19, further comprising a calibration (109) of the at least one nanotool (51, 52) so as to determine for example an elastic constant said at least one nanotool (51, 52).
FR1762934A 2017-12-22 2017-12-22 Nano-manipulation device and characterization method using such a device Pending FR3075983A1 (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020166976A1 (en) * 2001-05-08 2002-11-14 Masakazu Sugaya Beam as well as method and equipment for specimen fabrication
US20090000400A1 (en) * 2007-06-29 2009-01-01 Fei Company Method for attaching a sample to a manipulator
US20130023052A1 (en) * 2010-08-06 2013-01-24 Nobuaki Tanaka Manipulator system and manipulation method of micromanipulation target object
US20170030812A1 (en) * 2011-09-28 2017-02-02 Hysitron, Inc. Testing assembly including a multiple degree of freedom stage

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020166976A1 (en) * 2001-05-08 2002-11-14 Masakazu Sugaya Beam as well as method and equipment for specimen fabrication
US20090000400A1 (en) * 2007-06-29 2009-01-01 Fei Company Method for attaching a sample to a manipulator
US20130023052A1 (en) * 2010-08-06 2013-01-24 Nobuaki Tanaka Manipulator system and manipulation method of micromanipulation target object
US20170030812A1 (en) * 2011-09-28 2017-02-02 Hysitron, Inc. Testing assembly including a multiple degree of freedom stage

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
GÜNTER OXFORD INSTRUMENTS: "Omniprobe 400", 1 August 2012 (2012-08-01), XP055516718, Retrieved from the Internet <URL:https://nano.oxinst.com/assets/uploads/products/nanoanalysis/documents/Brochures/Omniprobe%20400.pdf> [retrieved on 20181018] *
KLEINDIEK GMBH: "NW-EM Nanoworkstattion", 1 January 2014 (2014-01-01), pages 1 - 5, XP055516697, Retrieved from the Internet <URL:https://www.kleindiek.com/fileadmin/public/brochures/nw-em.pdf> [retrieved on 20181018] *

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