Measurement apparatus for micro- and nano-scale material and measurement method thereof
10976238 ยท 2021-04-13
Assignee
Inventors
Cpc classification
International classification
Abstract
A measurement apparatus for micro- and nano-scale materials and a measurement method thereof are provided. The measurement apparatus for the micro- and nano-scale material includes a transmission electron microscope to generate a magnetic field, and a conductive flat punch and a sample which are arranged in the magnetic field. The sample includes the micro- and nano-scale materials. When the current passes through the sample and the conductive flat punch, the conductive flat punch deflects laterally relative to the sample with controllable displacement driven by the electromagnetic force. The required lateral displacement of the present invention is controllable, so that the utilization rate of equipment is greatly increased, and the cost is reduced. In addition, the whole test is performed in the transmission electron microscope, so that a measurement process can be observed in real time.
Claims
1. A measurement apparatus for a micro- and nano-scale material, comprising: a transmission electron microscope, used for generating a magnetic field in a first direction; a conductive flat punch, arranged on the magnetic field; a sample, arranged on the magnetic field, the sample comprising a micro- and nano-scale material, wherein the sample is electrically connected with the conductive flat punch to form an electric circuit, wherein the conductive flat punch has a first length at millimeter scale, and the sample has a second length and the second length of the sample is at micron-meter scale; a mechanical controller providing a load to the conductive flat punch to control a contact force between the conductive flat punch and the sample, wherein the load lasts 60 seconds at each time, and a value of the load is between 50 N and 200 N; and a current controller outputting a current which is increased at first and then decreased, wherein when a frictional property of the sample is tested, the current with a sine-wave is selected; and when a plastic deformation of the sample is tested, the current with an electric pulse is selected, wherein when the current passes through the sample and the conductive flat punch in a second direction, perpendicular to the first direction of the magnetic field; wherein the current has a peak value that is between 4 mA and 18 mA, and the current is increased at the interval of 2 mA, and the conductive flat punch deflects in a third direction perpendicular to the first and the second directions laterally in an amount from 0 nm to 440 nm relative to the sample with controllable displacement driven by an electromagnetic force that is in proportion to an intensity of the magnetic field and the current, thereby achieving measurements of static friction performance and kinetic friction performance of the sample; and wherein the conductive flat punch, the sample, the current controller and a current source meter are connected to each other in sequence.
2. The measurement apparatus for the micro- and nano-scale material of claim 1, wherein, the conductive flat punch is of a cantilever structure, and a free end of the cantilever structure is in contact with the sample.
3. The measurement apparatus for the micro- and nano-scale material of claim 1, wherein, the sample and the conductive flat punch is also connected in series with the current source meter and the current controller.
4. The measurement apparatus for the micro- and nano-scale material of claim 1, wherein, magnitude and/or frequency of the electromagnetic force is adjusted through current.
5. The measurement method using the measurement apparatus for the micro- and nano-scale material of claim 1, comprising first step (S1), installing the conductive flat punch and the sample in the magnetic field, wherein the sample is in contact with the conductive flat punch; second step (S2), electrically connecting the sample with the conductive flat punch to form the electric circuit; and third step (S3), passing the current to enable the conductive flat punch to move transversely under an action of an ampere force.
6. The measurement method of claim 5, wherein, in the first step (S1), the sample processed using a focused ion beam is installed on an electromechanical coupling holder, and the electromechanical coupling holder is inserted into a transmission electron microscope which generates the magnetic field.
7. The measurement method of claim 5, wherein, in the first step (S1), when the sample is insulated, the sample is coated with a conductive layer.
8. The measurement method using the measurement apparatus for the micro- and nano-scale material of claim 2, comprising: first step (S1), installing the conductive flat punch and the sample in the magnetic field, wherein the sample is in contact with the conductive flat punch; second step (S2), electrically connecting the sample with the conductive flat punch to form the electric circuit; and third step (S3), passing the current to enable the conductive flat punch to move transversely under an action of an ampere force.
9. The measurement method using the measurement apparatus for the micro- and nano-scale material of claim 3, comprising: first step (S1), installing the conductive flat punch and the sample in the magnetic field, wherein the sample is in contact with the conductive flat punch; second step (S2), electrically connecting the sample with the conductive flat punch to form the electric circuit; and third step (S3), passing the current to enable the conductive flat punch to move transversely under an action of an ampere force.
10. The measurement method using the measurement apparatus for the micro- and nano-scale material of claim 4, comprising: first step (S1), installing the conductive flat punch and the sample in the magnetic field, wherein the sample is in contact with the conductive flat punch; second step (S2), electrically connecting the sample with the conductive flat punch to form the electric circuit; and third step (S3), passing the current to enable the conductive flat punch to move transversely under an action of an ampere force.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
(1) Various other advantages and benefits of the present invention will become clearer for those of ordinary skill in the art by reading detailed descriptions in the preferred specific implementation modes in the text below. Accompanying drawings of the description are merely used to indicate the objectives of the preferred implementation modes, but are not deemed as limitations to the present invention. Apparently, the accompanying drawings described below are merely some of the embodiments of the present invention, based on which other drawings may be obtained by those of ordinary skill in the art without any creative effort. In addition, in the whole drawings, same referential numerals represent same components.
(2) In the drawings:
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(27) The present invention is further explained below in combination with the accompanying drawings and the embodiments.
DETAILED DESCRIPTION
(28) Specific embodiments of the present invention will be described in more detail below with reference to the accompanying drawings. Although the specific embodiments of the present invention are displayed in the accompanying drawings, it should be understood that the present invention can be implemented in various forms and should not be limited by the embodiments described herein. On the contrary, these embodiments are provided to understand the present invention more thoroughly, and the scope of the present invention can be completely passed to those skilled in the art.
(29) It should be noted that some vocabularies are used in the description and claims to refer to specific assemblies. Those skilled in the art should understand that a technician may possibly name the same assembly with different nouns. In the description and claims, assemblies are distinguished on the basis of functional differences instead of noun differences. For example, the including or comprising mentioned in the whole description and the claims is an open phrase, so that it should be explained as including but not limited to. Subsequent descriptions in the description are preferred implementation modes of implementing the present invention, so that the descriptions are intended for general principles of the description, but not intended to limit the scope of the present invention. The protection scope of the present invention shall be defined by the attached claims.
(30) To facilitate understanding of the embodiments of the present invention, the specific embodiments will be further explained and described below in combination with the accompanying drawings which do not constitute limitations to the embodiments of the present invention.
(31) For better understandings,
(32) a transmission electron microscope, used for generating a magnetic field 1;
(33) a conductive flat punch 2, arranged on the magnetic field 1; and
(34) a sample 3, arranged on the magnetic field 1, the sample 3 comprising the micro- and nano-scale material.
(35) When the current passes through the sample 3 and the conductive flat punch 2, the current direction is perpendicular to that of the magnetic field, and the conductive flat punch 2 generates a predetermined lateral displacement under the electromagnetic field.
(36) For further understandings of the present invention, in one embodiment, the conductive flat punch 2 is a driving unit. The effective length of the conductive flat punch 2 in the magnetic field is much greater than the length of the sample 3. It is known that the magnitude of an ampere force is in proportion to the intensity of the magnetic field, the magnitude of the current and the length of an energizing conductor. The conductive flat punch 2 is connected in series with the sample 3, so that the current flowing through is equal. The conductive flat punch 2 and the sample 3 are located in the same magnetic field, so that the intensity of the magnetic field is equal. The effective length of the conductive flat punch 2 in the magnetic field is at millimeter scale, and the length of the sample 3 is at micron-meter scale. Therefore, the ampere force on the conductive flat punch 2 is three orders of magnitude than that on the sample 3, and then when the conductive flat punch 2 is in contact with the sample 3, the ampere force on the sample 3 may be neglected.
(37) In the preferred embodiment of the measurement apparatus for the micro- and nano-scale material, the conductive flat punch is of a cantilever structure, and the free end of the cantilever structure is in contact with the sample.
(38) In the preferred embodiment of the measurement apparatus for the micro- and nano-scale material, the length of the conductive flat punch in the magnetic field is much greater than that of the sample. In one embodiment, the words much greater than mean that at least one magnitude greater than. The length of the conductive flat punch is at the millimeter scale, and the length of the sample is at the micron-meter scale.
(39) A series circuit of the sample and the conductive flat punch is also connected in series with a switch and a current controller 7.
(40) In the measurement apparatus for the micro- and nano-scale material, the magnitude and/or frequency of the transverse acting force is adjusted through the current.
(41) In the preferred embodiment of the measurement apparatus for the micro- and nano-scale material, a series circuit of the sample and the conductive flat punch is also connected in series with a current source meter 6 and a current controller 7.
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(43) a magnetic field generation unit, used for generating a magnetic field 1;
(44) a conductive flat punch 2, arranged on the magnetic field 1; and
(45) a sample 3, arranged on the magnetic field 1, the sample 3 comprising the micro- and nano-scale material.
(46) When the current passes through the sample 3 and the conductive flat punch 2, the current direction is perpendicular to that of the magnetic field, and the conductive flat punch 2 generates a predetermined transverse acting force under the electromagnetic field to move laterally relative to the sample.
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(48) In the preferred embodiment of the measurement apparatus for the micro- and nano-scale material of the present invention, the measurement apparatus further includes a mechanical controller which applies a predetermined load to the sample through the conductive flat punch 2.
(49) In the preferred embodiment of the measurement apparatus for the micro- and nano-scale material of the present invention, the measurement apparatus includes an electromechanical coupling holder arranged in the magnetic field, and the conductive flat punch 2 is arranged on the electromechanical coupling holder.
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(51) In the preferred embodiment of the measurement apparatus for the micro- and nano-scale material of the present invention, the electromechanical coupling holder is arranged in the magnetic field along the y-axis direction of the transmission electron microscope. In testing, the micro- and nano-scale sample 3 is connected in series with the conductive flat punch 2 in the electromechanical coupling holder and the current source meter 6, and after a current along a z-axis direction is applied, an electromagnetic field is generated and enables the conductive flat punch 2 to be subjected to an ampere force along an x-axis direction. In addition, the current source meter 6 is electrically connected with the current controller 7.
(52) For further understandings of the present invention, the following examples are particularly exemplified.
Embodiment 1 Measure the Friction Performance of a Micro- and Nano-Scale Material
(53) Referring to
Embodiment 2 Test the Failure Behavior of a Cantilever Structure of the Micro- and Nano-Scale Material
(54) Referring to
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(56) first step S1, a conductive flat punch and a sample are installed in a magnetic field, wherein the sample is in contact with the conductive flat punch;
(57) second step S2, the sample is electrically connected with the conductive flat punch to form an electric circuit; and
(58) third step S3, a current is applied to enable the conductive flat punch to move transversely under the ampere force.
(59) In the preferred implementation mode of the measurement method of the present invention, in the first step S1, the sample processed using a focused ion beam is installed on an electromechanical coupling holder, and the electromechanical coupling holder is inserted into a transmission electron microscope which generates the magnetic field.
(60) In the preferred implementation mode of the measurement method of the present invention, in the first step S1, when the sample is insulated, the sample is coated with a conductive layer.
(61) In the preferred implementation mode of the measurement method of the present invention, in the third step S3, a mechanical controller applies a load to the conductive flat punch to control a contact force between the conductive flat punch and the sample. The load lasts 60 s at each time, and the value of the load is between 50 N and 200 N.
(62) In the preferred implementation mode of the measurement method of the present invention, in the third step S3, a current controller outputs a linear current which is increased at first and then decreased.
(63) In the preferred implementation mode of the measurement method of the present invention, the sample is a micro- and nano-scale sample. When a frictional property of the sample is tested, a sine-wave current is selected. When the plastic deformation of the sample is tested, an electric pulse is selected.
(64) In the preferred implementation mode of the measurement method of the present invention, the sample is of a cantilever structure, and the side surface of the conductive flat punch is in contact with the sample.
(65) In the preferred implementation mode of the measurement method of the present invention, an ampere force-based measurement method for the in situ mechanical property of a micro- and nano-scale material includes:
(66) first step, a micro- and nano-scale sample processed using a focused ion beam is installed on an electromechanical coupling holder which is inserted into a transmission electron microscope;
(67) second step, a current source meter, the micro- and nano-scale sample and a conductive flat punch 2 are electrically connected through conductive wires to form an electric circuit;
(68) third step, real-time observation is performed under an imaging mode of the transmission electron microscope, and the position of the conductive flat punch 2 is adjusted through a mechanical control system on the electromechanical coupling holder so as to enable the conductive flat punch 2 to be in contact with the micro- and nano-scale sample;
fourth step, an electric signal of the circuit where the flat punch 2 and the micro- and nano-scale sample are located is measured to ensure a good electric contact;
fifth step, a linear current which is increased at first and then decreased is applied through a current controller with 10 s, wherein the peak value of the linear current is between 4 mA and 18 mA, which increases at the interval of 2 mA; and
sixth step, at the beginning of the test, a mechanical controller applies a load to the conductive flat punch 2 to control a contact force between the conductive flat punch 2 and the micro- and nano-scale sample, wherein the load kept for 60 s at each time, and the value of the load is between 50 N and 200 N.
(69) In the transmission electron microscope, a high-intensity magnetic field of about 2 T exists in the vicinity of the pole piece, generated by the electromagnetic lens. Thus, once the current flows through the flat punch, an ampere force may be generated and may enable the conductive flat punch 2 to move.
(70) As shown in
(71) As the conductive flat punch 2 is subjected to the ampere force perpendicular to a magnetic field direction 1 and a current direction 4, and when the ampere force is greater than a static friction force from the micro- and nano-scale sample 3, the conductive flat punch 2 would slide relative to the micro- and nano-scale sample 3, as shown in
(72) In addition, as the ampere force is proportional to the magnitude of the current, the ampere force could be adjusted by the current. In the mechanical test of the micro- and nano-scale sample, the sliding friction force is proportional to the contact force between the conductive flat punch 2 and the sample, so that the friction force may be adjusted by controlling the contact force.
(73) Sliding displacements of the conductive flat punch 2 under different loads and different current conditions are tested, respectively, thus obtaining curves between the sliding displacement of the conductive flat punch 2 and the current under different loads, as shown in
(74) As the direction of the ampere force is determined by the current direction, the direction of the ampere force may be controlled through the current direction. When the sine-wave current is applied, it can be observed that the flat punch reciprocates along the x axis.
(75) The frequency of the ampere force is also directly determined by the frequency of the current. When a sine-wave current of different periods is applied, it can be observed that the frequency of the sliding displacement of the flat punch is completely consistent with the frequency of the sine-wave current.
(76) In the transmission electron microscope, the magnitude of the ampere force also could be altered by changing the strength of the magnetic field.
(77) The present invention is further described through the following embodiments: according to the following embodiments, the present invention may be better understood. However, those skilled in the art easily understand that specific material ratios, process conditions and results that are described in the embodiments are merely used to describe the present invention, and should and may not restrict the present invention described in detail in claims.
Embodiment 3
(78) An ampere force-based measurement method for the friction force of a micro- and nano-scale material includes
(79) first step, a polycrystalline silver square pillar having an edge length of 3 m is processed using a focused ion beam, and the pillar shall be as short and thick as possible to guarantee relatively high stiffness and avoid bending along with the swinging of the flat punch;
second step, in the transmission electron microscope JEOL 2100F, the electromechanical coupling holder PI 95 ECR of the Hysitron Company is used to complete an electromechanical coupling experiment, the position of a tungsten flat punch is adjusted to contact with the top of the polycrystalline silver pillar, and an electrical test is performed to guarantee a good electric contact; and
third step, the mechanical controller is used to set a loading curve, and the load is maintained at 200 N for 60 s; during the constant load, a sine-wave current as shown in
(80) In the test process, it is observed that the flat punch slides relative to the silver pillar. The sliding displacement is linearly dependent on the current, and the frequency of the sliding displacement is completely consistent with the frequency of the sine-wave current.
(81) After the test, a scanning electron microscope is used for characterization. The morphology of the silver pillar subjected to scratching is as shown in
(82) The present embodiment indicates that the present invention may be used for in situ friction test on the micro- and nano-scale material, and the friction frequency is completely controlled by the frequency of the current.
Embodiment 4
(83) Apply a cyclic load to a cantilever structure through an electric pulse includes:
(84) first step, the cantilever 14 parallel to the current direction 4 is processed on a polycrystalline silver film by a focused ion beam, as shown in
second step, the flat punch is adjusted to contact with the needle-like structure at the top and contact with cantilever at the side as shown in
third step, specific parameters of electromechanical coupling are as shown in
(85) In the experiment, it can be observed that when the electric pulse is imposed, the flat punch slides laterally to deform the cantilever. As shown in
INDUSTRIAL PRACTICABILITY
(86) The measurement apparatus for the micro- and nano-scale material and the measurement method of the present invention may be manufactured and used in the field of micro- and nano-scale measurement.
(87) The basic theory of the present application is described above in combination with the specific embodiments. However, it should be noted that the advantages, benefits and effects that are mentioned in the present application are merely exemplary but not restrictive, and shall not be deemed as necessary for all the embodiments of the present application. In addition, the above-mentioned disclosed specific details are merely used as examples and to facilitate the understandings, but are not restrictive. The above-mentioned details do not limit that the present application must be implemented by the above-mentioned specific details.
(88) Block diagrams of devices, apparatuses, equipment and systems in the present application are merely used as exemplary examples, and are not intended to require or imply that these devices, apparatuses, equipment and systems must be connected, arranged and configured according to modes as shown in the block diagrams. Those skilled in the art will realize that these devices, apparatuses, equipment and systems may be connected, arrayed and configured in any way. For example, words such as including, comprising and having are open phrases meaning including but not limited to, and may be used interchangeably. Unless otherwise defined in the context, words or and and used herein mean a phrase and/or, and may be used interchangeably. The word for example used herein means a phrase for example but not limited to, and may be used interchangeably.
(89) It should be further noted that in the apparatus, equipment and method of the present application, each component or each step may be exploded and/or recombined. The exploding and/or recombination shall be deemed as equivalent solutions of the present application.
(90) The above descriptions of the disclosed aspects are provided to enable any one skilled in the art to make or use the present application. Various modifications to these aspects are particularly obvious to those skilled in the art, and general theories defined herein may be applied to other aspects without departing from the scope of the present application. Therefore, the present application is not intended to be limited to the aspects described herein, but shall fall within the widest scope consistent with the theories and novel features that are disclosed herein.
(91) For exemplification and description, the above descriptions that are not intended to limit the embodiments of the present application to the forms disclosed herein have been provided. Multiple exemplary aspects and embodiments have been discussed above, but those skilled in the art still will realize some deformations, modifications, changes, additions and sub combinations of the aspects and the embodiments.