CN109725005B - Transmission electron microscope sample rod head and transmission electron microscope sample rod applying same - Google Patents
Transmission electron microscope sample rod head and transmission electron microscope sample rod applying same Download PDFInfo
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- CN109725005B CN109725005B CN201711032623.7A CN201711032623A CN109725005B CN 109725005 B CN109725005 B CN 109725005B CN 201711032623 A CN201711032623 A CN 201711032623A CN 109725005 B CN109725005 B CN 109725005B
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Abstract
Transmission electron microscope sample pole head and use its sample pole, wherein transmission electron microscope sample pole head includes: a friction generator and a charge-pump assembly, wherein: the friction generator is used for generating electric charge; the charge excitation assembly is configured to receive a charge to provide excitation electrical energy to a sample disposed therein. Transmission electron microscope sample pole includes: the transmission electron microscope sample club head comprises a transmission electron microscope sample club body and at least one transmission electron microscope sample club head; wherein, the transmission electron microscope sample rod body is connected with the transmission electron microscope sample rod head through a bolt, a micro flange and the like; the transmission electron microscope sample rod head can be replaced by a piezoelectric ceramic motor-driven or fluid-driven triboelectrification rod head according to an experimental mode. Therefore, the sample rod provided by the disclosure can realize research on the friction layer material and the sample material of the friction generator, observe the change of the structure, the appearance and the electronic state of the friction layer material under the conditions of charge and no charge output, and the structure, the appearance and the electronic state characteristics of the sample under the conventional and electric excitation conditions.
Description
Technical Field
The disclosure belongs to the field of in-situ research of transmission electron microscope accessories and nano materials, and particularly relates to a transmission electron microscope sample rod head and a transmission electron microscope sample rod applying the transmission electron microscope sample rod head.
Background
The in-situ transmission electron microscope sample rod greatly widens the research field of the transmission electron microscope, the disclosing and developing of the friction generator provides bright prospect for green energy, and provides possibility for the collection and utilization of trace energy, particularly low-frequency energy, but an in-situ means is lacked at present, and the change mechanism of the friction layer of the friction generator in the working process is clearly researched.
The transmission electron microscope sample rod which is commercialized at present can provide bias voltage for a sample and electrically excite the sample. The in-situ gas and liquid environment sample rod can be used for researching various changes of samples in gas and liquid environments (including the condition of applying an electric field), and can also be used for researching the synthesis and catalytic reaction processes in situ. In addition, the materials and electrodes of the friction layer of the friction generator can be independently studied by using a conventional transmission mirror. However, the existing sample rod has the following defects in situ: 1. the existing sample rod usually provides bias voltage for a sample through an external circuit, so that the charge quantity applied to the sample cannot be accurately controlled, and the excitation and detection sensitivity to the sample is not high; 2. the structure and the appearance of a friction layer and an electrode material of a friction generator cannot be studied in situ by using a transmission electron microscope in the conventional sample rod; the structure, the appearance and the electronic state change of the material of the friction layer of the friction generator under the conditions of charge and charge output cannot be disclosed; 3. the club head and the club body of the prior sample club are generally integrated, and a new sample club needs to be purchased if an in-situ experiment is carried out by other means in the experiment process.
BRIEF SUMMARY OF THE PRESENT DISCLOSURE
Based on the above problems, a primary objective of the present disclosure is to provide a transmission electron microscope sample rod head and a transmission electron microscope sample rod using the same, for solving at least one of the above technical problems.
In order to achieve the above object, as one aspect of the present disclosure, the present disclosure proposes a transmission electron microscope sample club head comprising a friction generator and a charge excitation assembly, wherein: a friction generator for generating an electrical charge; a charge excitation assembly for receiving a charge to provide excitation electrical energy to a sample placed therein.
In some embodiments of the present disclosure, the above friction generator comprises: the first friction layer and the second friction layer are oppositely arranged; the first electrode layer is arranged on one side, away from the second friction layer, of the first friction layer; the second electrode layer is arranged on one side, away from the first friction layer, of the second friction layer; the two electrode layers are connected to two sides of a sample placed on the charge exciting assembly through leads and used for conducting charges to the charge exciting assembly so as to provide exciting electric energy for the sample.
In some embodiments of the present disclosure, a total width of the first friction layer and the first electrode layer and a total width of the second friction layer and the second electrode layer in a direction perpendicular to the electron beam are 200nm to 1.5 mm.
In some embodiments of the present disclosure, the first friction layer and the second friction layer generate electric charges by sliding friction; or the first friction layer and the second friction layer generate electric charges by a change in contact/separation state.
In some embodiments of the present disclosure, the triboelectric generator described above comprises a single electrode mode, i.e. one of the first electrode layer and the second electrode layer is grounded through the tem bar.
In some embodiments of the present disclosure, the rubbing surface of the first rubbing layer or the second rubbing layer is parallel to a direction of an electron beam, and the electron beam can penetrate through either the first rubbing layer or the second rubbing layer; preferably, the first friction layer and/or the second friction layer are replaceable structures.
In some embodiments of the present disclosure, the thickness of the first friction layer and/or the second friction layer in the electron beam direction is less than 100 nm.
In some embodiments of the present disclosure, one of the first friction layer and the second friction layer is fixed; the transmission electron microscope sample pole head still includes: a piezoelectric ceramic motor; and a driving probe connected to one end of the piezoelectric ceramic motor for driving the other of the first friction layer and the second friction layer to slide and rub against or change a contact/separation state with respect to the other of the first friction layer and the second friction layer.
In some embodiments of the present disclosure, the transmission electron microscope sample club head further includes: and one end of the first electrode lead is connected to the piezoelectric ceramic motor and used for supplying power to the piezoelectric ceramic motor.
In some embodiments of the present disclosure, one of the first friction layer and the second friction layer is fixed; the transmission electron microscope sample pole head still includes: a first gas-liquid inflow pipe for inflow of a fluid, and a first gas-liquid outflow pipe for outflow of the fluid; wherein, through the inflow and outflow of the fluid, drive another one of first friction layer and second friction layer to slide and rub or change the contact/separation state relative to one of them.
In some embodiments of the present disclosure, one of the first friction layer and the second friction layer is a flexible material for changing a contact/separation state with the other of the first friction layer and the second friction layer.
In some embodiments of the present disclosure, the transmission electron microscope sample club head further includes: the sample pool is used for containing a sample; the first gas inflow pipeline and the first gas outflow pipeline are divided into two paths, wherein the first path is communicated to the friction generator to provide fluid for driving the friction layer, and the second path is communicated to the sample pool to provide a sample.
In order to achieve the above object, as another aspect of the present disclosure, the present disclosure proposes a tem sample club head including a triboelectric generator that is permeable to an electron beam of a tem, comprising: the first friction layer and the second friction layer are oppositely arranged; the first electrode layer is arranged on one side, away from the second friction layer, of the first friction layer; the second electrode layer is arranged on one side, away from the first friction layer, of the second friction layer; the friction contact surfaces of the first friction layer and the second friction layer are parallel to an electron beam of a transmission electron microscope, and at least one of the first friction layer and the second friction layer is of a replaceable structure.
In some embodiments of the present disclosure, at least one of the combination of the first friction layer and the first electrode layer and the combination of the second friction layer and the second electrode layer is a replaceable structure.
In some embodiments of the present disclosure, the thickness of the first friction layer or the second friction layer in the electron beam direction is less than 100 nm.
In order to achieve the above object, as yet another aspect of the present disclosure, the present disclosure proposes a transmission electron microscope sample rod comprising: a transmission electron microscope sample rod body; and at least one of the transmission electron microscope sample club heads; the transmission electron microscope sample rod body is connected with the transmission electron microscope sample rod head through bolts, screws, locking jackscrews or a miniature sealing flange.
In some embodiments of the present disclosure, the transmission electron microscope sample club head further includes: a piezoelectric ceramic motor; and a driving probe connected to one end of the piezoelectric ceramic motor for driving one of the first friction layer and the second friction layer to slide relatively to the other one of the first friction layer and the second friction layer or to change a contact/separation state; one end of the first electrode lead is connected to the piezoelectric ceramic motor and used for supplying power to the piezoelectric ceramic motor; one end of the electrode slot is connected with the first electrode lead; the transmission electron microscope sample rod body comprises: and one end of the second electrode lead is connected to the power supply, and the other end of the second electrode lead is inserted into the electrode slot.
In some embodiments of the present disclosure, the transmission electron microscope sample club head further includes: a first gas inflow conduit for inflow of a fluid; and a first gas-liquid outflow conduit for outflow of a fluid; one of the first friction layer and the second friction layer is driven to slide and rub or change a contact/separation state relative to the other friction layer through inflow and outflow of the fluid; the transmission electron microscope sample rod body further comprises: a second gas-liquid inflow pipeline, one end of which is communicated with the first gas-liquid inflow pipeline and is used for providing fluid for the first gas-liquid inflow pipeline; and one end of the second gas-liquid outflow pipeline is communicated to the first gas-liquid outflow pipeline and is used for discharging fluid discharged by the second gas-liquid outflow pipeline.
The transmission electron microscope sample rod head and the transmission electron microscope sample rod using the same have the following beneficial effects:
1. the rod head comprises a friction generator and a charge excitation assembly, the sample is excited by charges generated by the friction generator, and the charge amount generated by the friction generator can be accurately controlled, so that the charge amount for exciting the sample can be controlled, the observation process is more convenient and the observation result is more sensitive to the sample sensitive to excitation;
2. due to the fact that the friction generator is adopted, one friction layer is driven to slide and rub or the contact/separation state of the friction layer is changed relative to the other friction layer through the piezoelectric ceramic motor or fluid, and therefore under a transmission electron microscope, the material change in the friction electrification process can be observed, the sample rod provided by the disclosure can simultaneously achieve research on materials of the friction layer of the friction generator and materials of the sample, and the structure, the appearance and the electronic state change of the materials under the conditions of charge and no charge output can be observed;
3. the pole body passes through modes such as bolt with the pole head and is connected, and wherein, the pole head can be piezoelectric ceramic motor drive friction electrification's structure and fluid drive friction electrification's structure, consequently when changing the experimental mode, can directly change the pole head, need not to purchase different sample poles again, and it is convenient to use more economy.
Drawings
Fig. 1 is a schematic view of an overall structure of a transmission electron microscope sample rod according to an embodiment of the present disclosure.
Fig. 2 is a schematic structural diagram of the inside of a rod of a sample for a transmission electron microscope according to an embodiment of the present disclosure.
Fig. 3(a) is a schematic structural view of a transmission electron microscope sample club head driven by a piezoelectric ceramic motor according to an embodiment of the present disclosure.
FIG. 3(b) is a schematic structural view of a friction generator of the TEM sample club head in FIG. 3(a) for generating electricity by sliding friction.
FIG. 3(c) is a schematic structural diagram of a friction generator of a TEM sample club head driven by a piezoelectric ceramic motor, which generates electricity by changing the contact/separation state.
Fig. 4(a) is a schematic structural view of a head of a sample fluidic-driven tem club according to an embodiment of the present disclosure.
FIG. 4(b) is a schematic diagram of the internal structure of the TEM sample club head in FIG. 4 (a).
FIG. 4(c) is a schematic sectional view of the transmission electron microscope sample club head of FIG. 4(a) from above.
FIG. 4(d) is a schematic structural view of the friction layer of the triboelectric generator inside the head of the TEM sample rod in FIG. 4 (a).
Fig. 5(a) is a schematic diagram of a transmission electron microscope sample rod used in studying a gas ionization or gas catalysis reaction process according to an embodiment of the disclosure.
Fig. 5(b) is a schematic diagram of a transmission electron microscope sample rod according to an embodiment of the present disclosure in use for studying a triboelectric input (lithium ion battery) electrochemical reaction process.
[ description of reference ]
10-a transmission electron microscope sample rod; 100-transmission electron microscope sample rod body;
200-transmission electron microscope sample rod head; 101-gas-liquid pipeline interface;
102-sample rod grab handle; 103-a first locator pin;
104-a first sealing ring; 105-a second locating pin;
106-electrode plug; 107-connecting and fixing screw holes;
108-gas liquid conduit port; 109-a second gas-liquid inflow pipe;
110-a second gas-liquid outflow conduit; 111-a second electrode lead;
112-a second sealing ring; 201-cylindrical interface;
202-a charge-pumping assembly; 203-a friction generator;
204-shaft head connecting screw; 205-electrode slots;
206-a first electrode lead; 207-piezoelectric ceramic motor drive;
208-frictional layer securing bars; 209-a first electrode of the charge pumping assembly;
210-a second electrode of the charge pumping arrangement; 211-piezo ceramic motor driven probe;
212-gas-liquid pipeline sealing blind plate; 213-first friction layer electrode;
214-a first friction layer; 215-second friction layer;
216-a second friction layer electrode; 217-sealing cover of the club head;
218-cover set screws; 219 — first gas inflow conduit;
220-a first gas-liquid outflow conduit; 221-a first external electrode;
222-a second external electrode; 223-a third sealing ring;
224-a fourth seal ring; 225-a silicon layer;
226-silicon nitride film; 227-supporting metal posts for upper and lower chips;
228-battery positive electrode; 229-battery negative electrode.
Detailed Description
For the purpose of promoting a better understanding of the objects, aspects and advantages of the present disclosure, reference is made to the following detailed description taken in conjunction with the accompanying drawings.
The utility model discloses a transmission electron microscope sample rod head, including friction generator and charge excitation subassembly, wherein: the friction generator is used for generating electric charge; the charge excitation assembly is configured to receive a charge to provide excitation electrical energy to a sample disposed therein.
Therefore, the sample is excited by the electric charge generated by the friction generator, and the electric charge generated by the friction generator can be accurately controlled, so that the electric charge for exciting the sample can be controlled, and for the sample sensitive to excitation, the observation process is more convenient and the observation result is more sensitive.
In some embodiments of the present disclosure, the above friction generator comprises: the first friction layer and the second friction layer are oppositely arranged; the first electrode layer is arranged on one side, away from the second friction layer, of the first friction layer; the second electrode layer is arranged on one side, away from the first friction layer, of the second friction layer; the two electrode layers are connected to two sides of a sample placed on the charge exciting assembly through leads and used for conducting charges to the charge exciting assembly so as to provide exciting electric energy for the sample.
In some embodiments of the present disclosure, a total width of the first friction layer and the first electrode layer and a total width of the second friction layer and the second electrode layer in a direction perpendicular to the electron beam are 200nm to 1.5 mm.
In some embodiments of the present disclosure, the first friction layer and the second friction layer generate electric charges by sliding friction; or the electric charge is generated by the change of the contact/separation state.
In some embodiments of the present disclosure, the triboelectric generator comprises a single-electrode mode, i.e. one of the first electrode layer and the second electrode layer is grounded via the tem bar.
In some embodiments of the present disclosure, the rubbing surface of the first rubbing layer or the second rubbing layer is parallel to a direction of an electron beam, and the electron beam can penetrate through either the first rubbing layer or the second rubbing layer; preferably, the first friction layer and/or the second friction layer are replaceable structures.
In some embodiments of the present disclosure, the thickness of the first friction layer and/or the second friction layer in the electron beam direction is less than 100 nm.
In some embodiments of the present disclosure, one of the first friction layer and the second friction layer is fixed; the transmission electron microscope sample pole head still includes: a piezoelectric ceramic motor; and a driving probe connected to one end of the piezo-ceramic motor for driving one of the first friction layer and the second friction layer to slide relatively to the other one of the first friction layer and the second friction layer or to change a contact/separation state.
In some embodiments of the present disclosure, the transmission electron microscope sample club head includes: and one end of the first electrode lead is connected to the piezoelectric ceramic motor and used for supplying power to the piezoelectric ceramic motor.
In some embodiments of the present disclosure, one of the first friction layer and the second friction layer is fixed; the transmission electron microscope sample pole head still includes: a first gas-liquid inflow pipe for inflow of a fluid, and a first gas-liquid outflow pipe for outflow of the fluid; wherein, through the inflow and outflow of the fluid, drive another one of first friction layer and second friction layer to slide and rub or change the contact/separation state relative to one of them.
As can be seen from the above description, the friction generator is adopted in the present disclosure, and one friction layer is driven by the piezoelectric ceramic motor or the fluid to slide and rub or change the contact/separation state relative to the other friction layer, so that under a transmission electron microscope, the observation of the material change in the triboelectrification process can be performed.
In some embodiments of the present disclosure, one of the first friction layer and the second friction layer is a flexible material for changing a contact/separation state with the other of the first friction layer and the second friction layer.
In some embodiments of the present disclosure, the tem sample club head further comprises a sample cell for holding a sample; the first gas inflow pipeline and the first gas outflow pipeline are divided into two paths, wherein the first path is communicated to the friction generator to provide fluid for driving the friction layer, and the second path is communicated to the sample pool for research.
The utility model also discloses a transmission electron microscope sample rod head, including friction generator, this friction generator permeable transmission electron microscope's electron beam includes: the first friction layer and the second friction layer are oppositely arranged; the first electrode layer is arranged on one side, away from the second friction layer, of the first friction layer; the second electrode layer is arranged on one side, away from the first friction layer, of the second friction layer; the friction contact surfaces of the first friction layer and the second friction layer are parallel to an electron beam of a transmission electron microscope, and at least one of the first friction layer and the second friction layer is of a replaceable structure.
The present disclosure also discloses a transmission electron microscope sample rod, including: the transmission electron microscope sample club head comprises a transmission electron microscope sample club body and at least one transmission electron microscope sample club head; the transmission electron microscope sample rod body is connected with the transmission electron microscope sample rod head through bolts, screws, locking jackscrews or a miniature sealing flange and the like. The screw is adopted for connecting the rod head and the rod body under the condition of fluid driving, and the blind plate and the sealing ring are used for sealing connection.
In some embodiments of the present disclosure, a transmission electron microscope sample shaft includes a first transmission electron microscope sample shaft head and a second transmission electron microscope sample shaft head; the first transmission electron microscope sample rod head and the second transmission electron microscope sample rod head are connected with the transmission electron microscope sample rod body in an interchangeable mode, wherein the first transmission electron microscope sample rod head is a transmission electron microscope sample rod head driven by a piezoelectric ceramic motor to generate friction electrification; the second TEM sample club head is a fluid-driven tribocharging TEM sample club head. Therefore, when the experiment mode is changed, the rod head can be directly replaced, different sample rods do not need to be purchased again, and the use is more economical and convenient.
In some embodiments of the present disclosure, the replaced tem sample club head is driven by a piezo-ceramic motor; at this time: the transmission electron microscope sample pole head still includes: a piezoelectric ceramic motor; and a driving probe connected to one end of the piezoelectric ceramic motor for driving one of the first friction layer and the second friction layer to slide relatively to the other one of the first friction layer and the second friction layer or to change a contact/separation state; one end of the first electrode lead is connected to the piezoelectric ceramic motor and used for supplying power to the piezoelectric ceramic motor; one end of the electrode slot is connected with the first electrode lead; transmission electron microscope sample pole body includes: and one end of the second electrode lead is connected to the power supply, and the other end of the second electrode lead is inserted into the electrode slot.
In some embodiments of the present disclosure, the replaced transmissive sample rod head is fluid driven; transmission electron microscope sample pole head still includes this moment: a first gas inflow conduit for inflow of a fluid; and a first gas-liquid outflow conduit for outflow of a fluid; one of the first friction layer and the second friction layer is driven to slide and rub or change a contact/separation state relative to the other friction layer through inflow and outflow of the fluid; transmission electron microscope sample pole body includes: a second gas-liquid inflow pipeline, one end of which is communicated with the first gas-liquid inflow pipeline and is used for providing fluid for the first gas-liquid inflow pipeline; and one end of the second gas-liquid outflow pipeline is communicated to the first gas-liquid outflow pipeline and is used for discharging fluid discharged by the second gas-liquid outflow pipeline.
In some embodiments of the present disclosure, the transmission electron microscope sample rod body comprises a hollow circular tube, in which the second gas-liquid inflow conduit, the second gas-liquid outflow conduit, and the second electrode lead are arranged.
In some embodiments of the present disclosure, the material of the first friction layer in the two friction generators includes an organic polymer material or an inorganic semiconductor material, and the organic polymer material may be polytetrafluoroethylene, polymethyl methacrylate, polyvinyl alcohol, polyester, polyisobutylene, or the like; the inorganic semiconductor material may be metal oxysulfide or indium tin oxide, etc.
In some embodiments of the present disclosure, the second friction layer of the two friction generators is fixed and transparent to the electron beam, and the material of the second friction layer includes a semiconductor material or a metal material, wherein the semiconductor material may be indium tin oxide, zinc oxide, tin sulfide, titanium dioxide, or other conventional semiconductor research materials, and the metal material may be aluminum, copper, gold, silver, or an alloy. Therefore, under a transmission electron microscope, the material change in the triboelectrification process can be observed, the research on the friction layer material and the sample material of the triboelectric generator can be realized simultaneously, and the change of the structure, the morphology and the electronic state of the material under the conditions of charge and no charge output can be observed.
In some embodiments of the present disclosure, the second friction layer of the two friction generators is a flexible and bendable deformation layer, the material of the second friction layer includes materials with different triboelectrification sequences (i.e. different electrification properties when in friction or contact separation) such as PET (polyethylene terephthalate), kapton (polyimide), PTE (polytetrafluoroethylene), polypropylene, etc. as compared with the first friction layer, at this time, the material of the second friction layer should also be transparent to the electron beam, so as to characterize the morphology and the change of the electronic state by means of contrast, electron energy loss spectrum, etc.; the first friction layer is made of a transparent material with respect to the electron beam, i.e. an inorganic material, and may be made of a metal material such as aluminum, copper, gold, silver or alloy, a semiconductor material such as indium tin oxide, zinc oxide, titanium dioxide or tin sulfide, or some other conventional semiconductor material, and the thickness of the first friction layer in the incident direction of the electron beam is controlled to be about 100 nm.
In some embodiments of the present disclosure, the transmission electron microscope sample rod may be used as an electrical sample rod, a mechanical sample rod, or a (fluid type) gas or liquid sample rod in a general sense, in addition to implementing the above-mentioned novel functions.
The transmission electron microscope sample rod provided by the present disclosure is described here as an example:
in some embodiments of the present disclosure, an in-situ TEM sample rod system is disclosed that allows real-time observation of triboelectric generation processes in a TEM and simultaneous observation of the process of excitation of the sample by the generated triboelectric charges.
The transmission electron microscope sample rod system comprises two parts, wherein one part is a transmission electron microscope sample rod body which contains an electric lead and a gas-liquid pipeline inside, and the other part is a transmission electron microscope sample rod head which can be mutually replaced and is driven by a piezoelectric ceramic motor to generate friction electrification and a transmission electron microscope sample rod head which is driven by gas and liquid fluid to generate friction electrification.
The transmission electron microscope sample rod head comprises two functional areas, wherein one functional area is a friction electrification functional area, and the other functional area is a functional area for exciting a sample by utilizing friction induced charges. The friction layers or the samples to be excited in the two functional areas are transparent to the electron beams, so that the electrification and excitation functions of the two functional modules can be observed or imaged in real time by using a transmission electron microscope, and the observation results of the two functional areas can be correlated.
The transmission electron microscope sample rod provided by the present disclosure is explained in detail by the following examples.
Examples
As shown in fig. 1, the present embodiment provides a tem sample shaft 10, which includes a tem sample shaft 100 and a replaceable tem sample shaft head 200.
Specifically, as shown in fig. 2, the shaft 100 of the tem sample rod 10 includes a gas-liquid pipe interface 101, a sample rod hand-holding handle 102, a first sealing ring 104, a first positioning pin 103 and a second positioning pin 105, wherein the inside of the rod of the sample rod is a hollow structure, and the inside of the rod includes a second gas-liquid inflow pipe 109, a second gas-liquid outflow pipe 110 and a second electrode lead 111.
The connecting part of the transmission electron microscope sample rod body 100 and the rod head 200 is provided with an electrode plug 106, a connecting and fixing screw hole 107, a gas-liquid pipeline port 108 and a second sealing ring 112, and the rod body and the rod head are connected and fixed by installing a rod body and rod head connecting screw 204 in the connecting and fixing screw hole 107.
The tem club head 200 includes a cylindrical interface 201 for connecting the club body, two regions transparent to the electron beam, i.e., a friction generator 203 and a charge exciting assembly 202 for exciting the sample by the charges generated by friction.
The tem sample club head 200 of this example has two types:
in the first club head 200, as shown in fig. 3(a), a club head electrode slot 205 is connected to a first electrode lead 206 of the club head to drive a piezo ceramic motor driving device 207, wherein a piezo ceramic motor driving probe 211 is connected to a friction generator (TENG) 203. The upper friction layer (i.e., the second friction layer 215 shown in fig. 3 (b)) of the friction generator 203 is fixed by the friction layer fixing rod 208 via the second friction layer electrode 216, and the lower friction layer (i.e., the first friction layer 214 shown in fig. 3 (b)) is movable back and forth via the first friction layer electrode 213 by the piezo-ceramic motor driving probe 211. The triboelectric generator 203 is connected with a first electrode 209 and a second electrode 210 of the charge excitation assembly, and is connected with two ends of the sample, so that the sample research under the condition of triboelectric excitation can be carried out. Wherein the friction generator may be replaced with a contact/separation type friction layer as shown in fig. 3 (c). When the first type of head is used, the gas-liquid pipe is sealed by the second packing 112 and the gas-liquid pipe sealing blank 212.
The material selection of the first friction layer, the second friction layer, the first electrode layer and the second electrode layer may be any material suitable for the existing friction generator, and is not limited to the present disclosure. For example, the first friction layer and the second friction layer may be made of a material such as a semiconductor or an insulator, or one of them may be made of a conductive material. The material of the first electrode layer and the second electrode layer may be an inorganic conductor or an organic conductor material.
Typical embodiments of this first head are: the piezoelectric ceramic motor driving device with large precession distance and high-frequency vibration is preferred, so that the friction layer is driven to generate higher power generation, and meanwhile, the piezoelectric ceramic motor driving device can provide more variable selection space for the research of a triboelectrification mechanism. The first friction layer 214 is made of polymer material such as teflon. The second friction layer 215 is fixed on the upper end of the friction power generation area, the material is electron beam transparent and has a structure or an electron state change under the action of polarization charges, the material of the second friction layer 215 is within the range of 500nm to 1mm in a plane perpendicular to the incidence plane of the electron beams, and the thickness along the direction of the electron beams is about 100nm so as to be convenient for the electron beams to transmit; the material of the second friction layer 215 is a semiconductor or a metal material, such as aluminum, which generates polarization charges by sliding friction with the first friction layer 214, depending on the material used and the experimental manner. The total width of the single friction layer plus electrode material of the first friction layer 214 and the second friction layer 215 should be controlled to be about 200nm to 1.5 mm.
In addition, the friction generator 203 can be made into a single-electrode mode, that is, one end of the electrode is connected to the transmission electron microscope sample rod, and the transmission electron microscope sample rod is used for grounding to study the change of the friction layer at the other end, that is, the electrode (the friction layer and the electrode are made of the same material).
The composite material of the friction layer and the electrode can be manufactured by a micro-machining or nano-machining process and fixed by FIB. The transmission electron microscope sample rod also comprises 2 observation windows, one observation window is a common sample observation window, the other observation window is positioned at the friction generator, and the performance of the friction layer material of the friction generator in a friction electrification state or an electric energy output state can be studied in situ. The first friction layer and/or the second friction layer are of replaceable structures, or at least one of the combination of the first friction layer and the first electrode layer and the combination of the second friction layer and the second electrode layer is of replaceable structures, and the thickness of the first friction layer or the second friction layer is smaller than 100nm along the direction of electron beams. In order to enable the friction layer material to be researched to reach an observable level, the thickness can be controlled by using a nano film growth method or preprocessing is carried out by using FIB (focused ion beam), the thickness requirement of being transparent to an electron beam, namely about 100nm, is ensured to be reached along the direction of the electron beam, and the size (friction functional area) in the direction vertical to the electron beam meets the space limitation of about 4mm of the rod head. The friction layer and the sample to be excited are fixed in the grooves connected with the two functional areas in an FIB processing mode, and after the research is finished, the friction layer and the electrodes can be removed by using FIB ion beams, so that the friction layer and the sample can be replaced. As shown in fig. 3(b), the piezo-ceramic motor driving probe 211 drives the first and second friction layers 214, 215 to slide relatively to generate frictional charges, and when the first and second friction layers 214, 215 move relatively to each other for a certain distance, induced charges are generated, and the first and second friction layer electrodes 213, 216 are connected to both sides of the sample to be observed through the wires of the first and second electrodes 209, 210 of the charge excitation assembly, so that an alternating current output with a constant total charge amount (determined by the surface area of the friction layers) can be formed, and thus, typical mechanical and electrical characteristics, etc. of the sample under the excitation of frictional electricity can be studied. In the implementation, the friction surface of the first friction layer or the second friction layer (namely the surface of one friction layer facing to the other friction layer) is parallel to the electron beam, and the observation surface of the friction layer is perpendicular to the electron beam, so that the generation process of triboelectrification and the corresponding change rule of the material morphology, the structure, the electron state and the like of the friction layer in the process can be simultaneously observed by utilizing characterization means such as a high-resolution phase contrast image or an electron energy loss spectrum and the like in the transmission electron mirror.
In other embodiments, there may be no other sample, and only one observation window is provided, and the friction layer in the friction generator may be used as a sample in the sample holder of the transmission electron microscope, and is used to in-situ study changes of the surface structure, the charge state, and the like of the material of the friction layer in the friction power generation process.
The second head and the operation mode are shown in fig. 4(a) to (d). Similarly, as shown in fig. 4(a), the tem sample club head 200 includes a friction generator 203 and a charge exciting assembly 202, the outer side of the club head is sealed by a sealing cover 217 and a sealing ring of the club head in a gas environment, and the sealing cover 217 of the tem sample club head 200 is fixed by a cover fixing screw 218. As shown in fig. 4(b), the club head is provided with a first gas-liquid inflow pipe 219 and a first gas-liquid outflow pipe 220, the gas (liquid) is divided into two branches after entering, one branch is used for driving the friction generator 203 driven by the fluid, and the other branch is used as a part of the sample for gas-liquid triboelectric ionization research. The triboelectric generator 203 may be as shown in fig. 4(d) in which there is a flexible, bendable deformable layer (i.e. the second friction layer 215) for contact separation. The schematic sectional view (from above) of the front end of the rod head is shown in fig. 4(c), wherein the friction generator 203 and the sample to be excited are both packaged in a sealed space surrounded by a sealed chip formed by a silicon layer 225, the sealed chip is fixed by a supporting metal column 227 of an upper chip and a lower chip, the friction generator 203 and the charge excitation assembly 202 are both sealed by a third sealing ring 223 and a fourth sealing ring 224 of the packaged chip, and the observation window of the chip is an amorphous structure SiN film 226 with a thickness of 30 nm. After the frictional charge is generated, the frictional charge is led out by the first external electrode 221 and the second external electrode 222 to provide excitation electric energy for gas ionization and electrochemical reaction, and in particular, in use, the connection of the club head is as shown in fig. 5(a) - (b).
Typical embodiments of this second head are:
1. by using a program-controlled injector with variable flow rate, pulse gas to be excited and researched is introduced through the first gas-liquid inflow pipe 219 to drive the friction layer sheets to be in continuous contact separation, so that friction charges and induced charges are generated, and after the pulse gas is introduced into the charge excitation assembly 202 through the first external electrode 221 and the second external electrode 222, as shown in fig. 5(a), a gas ionization process or a chemical reaction between a nano catalyst and the gas under the excitation of friction electricity and the like can be directly researched through an imaging or energy spectrum means. The thickness of a sample to be researched or an electrode plate is not too large and should be about 10-500 nm, the size in a plane perpendicular to an electron beam is not particularly equal to that of a rod head in the range of 1-3 mm, and the electrode plate can be fixed between two chips in a clamping groove mode. In addition, the sample should be placed between the upper and lower chips, and should not be too large. The sample cannot come into contact with the observation windows of the upper and lower chips.
2. Similarly, by using a programmable injector with variable flow rate, the liquid can be introduced into the rod head via the first gas inflow pipe 219 to drive the friction layer to contact and separate and generate induced charges, as shown in fig. 5(b), the induced charges are introduced into two ends of the lithium ion battery electrode, i.e. into the battery anode 228 and the battery cathode 229 of the lithium ion battery, and the outer end of the electrode of the friction layer should be isolated by a dielectric of an insulating layer to ensure the conduction of the charges. As shown in fig. 5(b), the morphology order/disorder structure change of the positive electrode 228 of the lithium ion battery during charging and discharging triboelectric is observed in situ in a transmission electron microscope. The material of the battery anode 228 here is preferably a nanostructure such as a nano conductor or a semiconductor nanowire, which may be a silicon (Si) nanowire, a gold (Au) nanowire, or the like, to allow electron beams to be observed by direct imaging.
It should also be noted that directional terms, such as "upper", "lower", "front", "rear", "left", "right", and the like, used in the embodiments are only directions referring to the drawings, and are not intended to limit the scope of the present disclosure. Throughout the drawings, like elements are represented by like or similar reference numerals. Conventional structures or constructions will be omitted when they may obscure the understanding of the present disclosure.
And the shapes and sizes of the respective components in the drawings do not reflect actual sizes and proportions, but merely illustrate the contents of the embodiments of the present disclosure. Furthermore, in the claims, any reference signs placed between parentheses shall not be construed as limiting the claim.
Unless otherwise indicated, the numerical parameters set forth in the specification and attached claims are approximations that can vary depending upon the desired properties sought to be obtained by the present disclosure. In particular, all numbers expressing quantities of ingredients, reaction conditions, and so forth used in the specification and claims are to be understood as being modified in all instances by the term "about". Generally, the expression is meant to encompass variations of ± 10% in some embodiments, 5% in some embodiments, 1% in some embodiments, 0.5% in some embodiments by the specified amount.
Furthermore, the word "comprising" does not exclude the presence of elements or steps not listed in a claim. The word "a" or "an" preceding an element does not exclude the presence of a plurality of such elements.
The use of ordinal numbers such as "first," "second," "third," etc., in the specification and claims to modify a corresponding element is not itself intended to imply any ordinal numbers for the element, nor the order in which an element is sequenced or methods of manufacture, but are used to distinguish one element having a certain name from another element having a same name, but rather, to distinguish one element having a certain name from another element having a same name.
In addition, unless steps are specifically described or must occur in sequence, the order of the steps is not limited to that listed above and may be changed or rearranged as desired by the desired design. The embodiments described above may be mixed and matched with each other or with other embodiments based on design and reliability considerations, i.e., technical features in different embodiments may be freely combined to form further embodiments.
Similarly, it should be appreciated that in the foregoing description of exemplary embodiments of the disclosure, various features of the disclosure are sometimes grouped together in a single embodiment, figure, or description thereof for the purpose of streamlining the disclosure and aiding in the understanding of one or more of the various disclosed aspects. However, the disclosed method should not be interpreted as reflecting an intention that: that is, the claimed disclosure requires more features than are expressly recited in each claim. Rather, as the following claims reflect, disclosed aspects lie in less than all features of a single foregoing disclosed embodiment. Thus, the claims following the detailed description are hereby expressly incorporated into this detailed description, with each claim standing on its own as a separate embodiment of this disclosure.
The above-mentioned embodiments are intended to illustrate the objects, aspects and advantages of the present disclosure in further detail, and it should be understood that the above-mentioned embodiments are only illustrative of the present disclosure and are not intended to limit the present disclosure, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present disclosure should be included in the scope of the present disclosure.
Claims (14)
1. A tem sample club head comprising: a friction generator and a charge-pump assembly, wherein:
the friction generator is used for generating electric charge; the friction generator includes:
the first friction layer and the second friction layer are oppositely arranged;
the first electrode layer is arranged on one side, away from the second friction layer, of the first friction layer; and
the second electrode layer is arranged on one side, far away from the first friction layer, of the second friction layer;
the first friction layer and the second friction layer generate the electric charges through sliding friction; alternatively, the first friction layer and the second friction layer generate the electric charges by a change in contact/separation state; the friction generator can penetrate through an electron beam of a transmission electron microscope, the friction contact surface of the first friction layer and the second friction layer is parallel to the electron beam of the transmission electron microscope, and the total width of the first friction layer and the first electrode layer and the total width of the second friction layer and the second electrode layer in the direction perpendicular to the electron beam are 200 nm-1.5 mm; the thickness of the first friction layer and/or the second friction layer along the direction of the electron beam is less than 100 nm;
the charge excitation assembly is used for receiving the charge to provide excitation electric energy for a sample placed in the charge excitation assembly.
2. The TEM sample club head of claim 1, wherein the two electrode layers are connected to two sides of the sample placed on the charge excitation member by wires for conducting the charges to the charge excitation member to provide excitation electrical energy to the sample.
3. The tem club head of claim 1, wherein the triboelectric generator comprises a single electrode mode, i.e., one of the first and second electrode layers is grounded through the tem.
4. The TEM sample club head as recited in any one of claims 1-3, wherein the first friction layer and/or the second friction layer is a replaceable structure.
5. The TEM sample club head as recited in any one of claims 1-3, wherein one of the first friction layer and the second friction layer is fixed;
the transmission electron microscope sample rod head further comprises:
a piezoelectric ceramic motor; and
and the driving probe is connected with one end of the piezoelectric ceramic motor and is used for driving the other one of the first friction layer and the second friction layer to slide and rub or change the contact/separation state relative to the other one of the first friction layer and the second friction layer.
6. The TEM sample club head of claim 5, further comprising:
and one end of the first electrode lead is connected to the piezoelectric ceramic motor and used for supplying power to the piezoelectric ceramic motor.
7. The TEM sample club head as recited in any one of claims 1-3, wherein one of the first friction layer and the second friction layer is fixed;
the transmission electron microscope sample rod head further comprises:
a first gas inflow conduit for inflow of a fluid, an
A first gas-liquid outflow conduit for outflow of the fluid;
wherein, through the inflow and outflow of the fluid, drive one of them another one of the first friction layer and second friction layer to slide and rub or change the contact/separation state relative to one of them.
8. The tem club head of claim 7, wherein one of the first friction layer and the second friction layer is a compliant material for changing a state of contact/separation with the other of the first friction layer and the second friction layer.
9. The tem sample club head of claim 8, further comprising:
a sample cell for holding the sample;
wherein the first gas inflow conduit and the first gas outflow conduit are equally divided into two paths, wherein the first path is communicated to the friction generator to provide the fluid for driving the friction layer, and wherein the second path is communicated to the sample cell to provide the sample.
10. A TEM sample club head comprising a triboelectric generator permeable to an electron beam of a TEM, comprising:
the first friction layer and the second friction layer are oppositely arranged;
the first electrode layer is arranged on one side, away from the second friction layer, of the first friction layer;
the second electrode layer is arranged on one side, far away from the first friction layer, of the second friction layer;
the first friction layer and the second friction layer generate electric charges through sliding friction; alternatively, the first and second electrodes may be,
the first friction layer and the second friction layer generate the electric charges by a change in contact/separation state;
the thickness of the first friction layer or the second friction layer along the direction of the electron beam is less than 100 nm;
the friction contact surfaces of the first friction layer and the second friction layer are parallel to the electron beam of the transmission electron microscope, and at least one of the first friction layer and the second friction layer is of a replaceable structure;
the total width of the first friction layer and the first electrode layer and the total width of the second friction layer and the second electrode layer in the direction perpendicular to the electron beam are 200 nm-1.5 mm.
11. The tem club head of claim 10, wherein at least one of the combination of the first friction layer and the first electrode layer and the combination of the second friction layer and the second electrode layer is a replaceable structure.
12. A transmission electron microscope sample holder, comprising:
transmission electron microscope sample rod body, and
at least one tem tip according to any one of claims 1 to 11;
the transmission electron microscope sample rod body is connected with the transmission electron microscope sample rod head through bolts, screws, locking jackscrews or a miniature sealing flange.
13. The TEM sample holder of claim 12, wherein,
the transmission electron microscope sample rod head further comprises:
a piezoelectric ceramic motor; and
the driving probe is connected with one end of the piezoelectric ceramic motor and is used for driving one of the first friction layer and the second friction layer to slide and rub or change a contact/separation state relative to the other friction layer;
a first electrode lead, one end of which is connected to the piezoelectric ceramic motor and is used for supplying power to the piezoelectric ceramic motor;
one end of the electrode slot is connected with the first electrode lead;
the transmission electron microscope sample rod body includes:
and one end of the second electrode lead is connected to a power supply, and the other end of the second electrode lead is inserted into the electrode slot.
14. The TEM sample holder of claim 12, wherein,
the transmission electron microscope sample rod head further comprises:
a first gas inflow conduit for inflow of a fluid; and
a first gas-liquid outflow conduit for outflow of the fluid;
driving one of the first friction layer and the second friction layer to slide and rub or change a contact/separation state relative to the other by inflow and outflow of the fluid;
the transmission electron microscope sample rod body still includes:
a second gas-liquid inflow pipe, one end of which is communicated to the first gas-liquid inflow pipe and is used for providing fluid for the first gas-liquid inflow pipe;
and one end of the second gas-liquid outflow pipeline is communicated to the first gas-liquid outflow pipeline and is used for discharging the fluid discharged by the first gas-liquid outflow pipeline.
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| CN114166674B (en) * | 2021-12-03 | 2024-01-30 | 中国地质大学（北京） | Device and method for testing interface abrasion of metal surface |
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