CN114225975A - Electron microscope fluid micro-element temperature control chip and manufacturing method thereof - Google Patents
Electron microscope fluid micro-element temperature control chip and manufacturing method thereof Download PDFInfo
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- CN114225975A CN114225975A CN202111370995.7A CN202111370995A CN114225975A CN 114225975 A CN114225975 A CN 114225975A CN 202111370995 A CN202111370995 A CN 202111370995A CN 114225975 A CN114225975 A CN 114225975A
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- B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
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- B01L3/502707—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by the manufacture of the container or its components
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Abstract
The invention relates to a method for manufacturing an electron microscope fluid micro element temperature control chip by ion beam etching and a product thereof, wherein the electron microscope fluid micro element temperature control chip comprises an upper piece and a lower piece, the upper piece and the lower piece are silicon substrates, the front surfaces of the upper piece and the lower piece are respectively provided with an insulating layer, the front surface of the upper piece and the front surface of the lower piece are fixedly bonded through a bonding layer, and the upper piece, the lower piece and the bonding layer form a cavity together; the upper piece is provided with a first window, the lower piece is provided with a heating electrode, a liquid inlet, a liquid outlet, a heating wire and a second window, and the heating wire is positioned in the second window; the electron microscope fluid infinitesimal temperature control chip provided by the invention can directly observe the appearance of the heating wire in the second window, can be used for measuring the local temperature change of the fluid and controlling the feedback temperature of the fluid infinitesimal, and is convenient for a user to better understand the thermal reaction process of the local position in the micron nanometer fluid solution, the interaction among the fluid infinitesimal and the influence of the temperature change of the infinitesimal part on the chemical reaction.
Description
Technical Field
The invention relates to the field of heating chips, in particular to an electron microscope fluid infinitesimal temperature control chip and a manufacturing method thereof based on ion beam etching for manufacturing the electron microscope fluid infinitesimal temperature control chip.
Background
The transmission electron microscope and the scanning electron microscope are collectively called as an electron microscope, and the ultra-high time resolution and spatial resolution of the electron microscope become effective means for people to characterize and observe materials, but the high-vacuum environment enables the electron microscope to only study some solid samples and ionic liquid with low saturated vapor pressure, the related application of the electron microscope in most of liquid and gas is greatly limited, the in-situ observation of the solution can be realized by people due to the occurrence of a silicon nitride liquid pool chip, and the in-situ observation of multi-physical-field coupling under the micro-scale can be realized by adding physical fields such as heat, electricity, light, force and the like to a silicon nitride liquid pool through the micro-nano processing technology by researchers.
The patent publication CN110501365A discloses a heating chip, which has several disadvantages, among which, the most important point is that the chip can only heat the whole observed area, and does not have the micro-area temperature detection function and the micro-area temperature heating function, which is not convenient for people to control the temperature of the micro-nano fluid in the fluid accurately.
Disclosure of Invention
The invention aims to provide an electron microscope fluid infinitesimal temperature control chip which can directly observe a heating wire and has the functions of fluid infinitesimal temperature control and detection.
The specific scheme is as follows:
an electron microscope fluid micro element temperature control chip comprises an upper chip and a lower chip, wherein the upper chip and the lower chip are single chips with specific functions manufactured by various micro-nano processing methods, the front and back of the upper sheet are provided with insulating layers, the front of the upper sheet and the front of the lower sheet are fixed through bonding layers, the upper sheet, the lower sheet and the bonding layers form a closed chamber together, the upper sheet is provided with a first window, the lower sheet is provided with a liquid injection port, an outflow port, a heating layer and a second window, the first window and the second window are arranged oppositely, fluid flows in through the liquid injection port, the outflow port flows out, the fluid is observed through the first window and the second window, the heating layer is also connected with a heating wire, the heating wires are in spiral ring shapes which are mutually reserved with gaps and are not connected, the heating wires are arranged in the second window, and the internal temperature of the fluid is controlled and monitored in real time through the heating wires.
Furthermore, the area occupied by the heating wires is not more than a square area with the length of three microns by three microns, the heating wires are positioned in the central area of the second window, and the gap between the heating wires is 20-200 nanometers.
Further, the heating layer comprises four contact electrodes, and the four contact electrodes form two pairs, wherein one pair is used as a heating electrode, and the other pair is used as a monitoring electrode.
Furthermore, the heating wire is manufactured by a material reducing process, the film material of the heating wire is subjected to film coating deposition in advance, and is accurately cut into spiral rings which are mutually provided with gaps in a high vacuum environment of a focused ion beam, the gaps are uniform and are not connected with each other.
Further, the heating wire is made of platinum, molybdenum, tungsten, gold, a semiconductor or a piezoelectric ceramic material.
The invention also provides a method for manufacturing the electron microscope fluid micro-element temperature control chip by ion beam etching, which comprises the following steps:
s1, processing a first window on the silicon substrate A with the insulating layer on the front and back surfaces to manufacture an upper wafer;
s2, processing four contact electrodes, a liquid inlet, a liquid outlet, a second window and heating wires on a silicon substrate B with insulating layers on the front and back surfaces, wherein the heating wires are in a spiral ring shape which is provided with gaps and is not connected with each other and are arranged in the second window to manufacture a lower piece;
and S3, fixing the upper sheet and the lower sheet through the bonding layer, and aligning the centers of the first window and the second window to obtain the electron microscope fluid micro element temperature control chip.
Further, step S2 includes:
s21, transferring the patterns of the second window, the liquid inlet and the liquid outlet from the photoetching mask plate to the back surface of the silicon substrate B with insulating layers on the front and back surfaces by adopting a photoetching process, developing in a positive photoresist developing solution, and washing with deionized water to obtain a silicon substrate B1;
s22, removing the insulating layer corresponding to the liquid inlet, the liquid outlet and the second window on the back of the silicon substrate B1 by adopting a reactive ion etching or ion beam etching process, and then soaking in an acetone solution to remove the photoresist to obtain a silicon substrate B2;
s23, putting the silicon wafer into a KOH solution or a tetramethylammonium hydroxide solution by adopting a wet etching process, removing the substrate silicon corresponding to the liquid inlet, the liquid outlet and the second window of the silicon substrate B2, then soaking and washing the silicon substrate B2 with an acid solution, and washing the silicon substrate with deionized water to obtain a silicon substrate B3;
s24, transferring the heating electrode and the rectangular position pattern with the predicted heating wire etched on the window from the photoetching mask plate to the front surface of the silicon substrate B3 by adopting an ultraviolet photoetching or laser direct writing photoetching process, developing in positive photoresist developing solution, and washing with deionized water to obtain a silicon substrate B4;
s25, sputtering a heating material film on the front surface of a silicon substrate B4 by adopting a direct current magnetron sputtering, thermal evaporation coating or electron beam evaporation coating process, connecting electrodes through a square metal film with the diameter not more than 5 microns by 5 microns, soaking the electrodes with acetone to remove the photoresist and the metal film on the photoresist, and washing with deionized water to obtain a silicon substrate B5;
s26: carrying out laser scribing on the silicon substrate B5 to obtain a single chip B6;
s27: and removing redundant heating membrane filaments at the position of the heating filament on the single sheet B6 by adopting a focused ion beam ion etching process, and transferring the pattern of the heating filament to a window to obtain a lower sheet.
Further, the photolithography process adopted in step S21 is: and (3) exposing in a hard contact mode of an ultraviolet lithography machine, wherein the developing time is 45 seconds, and the exposing time is 10-30 seconds.
Further, the reactive ion etching process adopted in step S22 is as follows: the etching rate is 10-20 nanometers per second, and the etching time is 10-120 seconds.
Further, the wet etching process adopted in step S23 is as follows: and (3) etching by using a potassium hydroxide solution with the mass percentage concentration of 20-50%, wherein the etching temperature is 60-100 ℃, and the etching time is 2-4 hours.
Further, the photolithography process adopted in step S24 is: and (3) exposing in a hard contact mode of an ultraviolet lithography machine, wherein the developing time is 45 seconds, and the exposing time is 10-30 seconds.
Further, the coating process adopted in step S25 is as follows: the vacuum degree reaches 7.6 x 10-5, a 3-10 nanometer titanium film is sputtered to serve as an adhesive layer, a 100-300 nanometer metal film is sputtered to serve as a heating wire, and the metal film can be made of materials such as platinum, molybdenum, tungsten, gold, semiconductors, piezoelectric ceramics and the like.
Further, the focused ion beam etching process adopted in step S27: bombarding and etching with gallium ion beam at current of 10-20pA and residence time of 10-15 μ S, and repeating for 5-7 times.
Compared with the prior art, the electron microscope fluid micro element temperature control chip provided by the invention has the following advantages: the electron microscope fluid micro element temperature control chip provided by the invention adopts a plurality of photoetching technologies and other processing technologies to realize seamless combination of millimeter-to-micron and nanometer level micro area structures, and superposes a focused ion beam imaging and processing method to accurately introduce the fluid micro element and control the temperature of a micro-nano area, so that the measurement of the local temperature change of the fluid and the feedback temperature control of the fluid micro element can be realized, and the chip has an important promotion effect on the research of the thermal reaction process and the mass transfer in the nanometer level micro field.
Drawings
Fig. 1 shows a schematic view of a silicon substrate.
FIG. 2 shows a schematic cross-sectional view of an electron microscopy fluid micro-element temperature control chip.
Fig. 3 shows a schematic view of the upper sheet.
Fig. 4 shows a schematic view of the lower sheet.
Fig. 5 shows an enlarged view of the heating wire.
Detailed Description
To further illustrate the various embodiments, the invention provides the accompanying drawings. The accompanying drawings, which are incorporated in and constitute a part of this disclosure, illustrate embodiments of the invention and, together with the description, serve to explain the principles of the embodiments. Those skilled in the art will appreciate still other possible embodiments and advantages of the present invention with reference to these figures. Elements in the figures are not drawn to scale and like reference numerals are generally used to indicate like elements.
The invention will now be further described with reference to the accompanying drawings and detailed description.
Example 1
As shown in fig. 1 to 5, an electron microscope fluid micro element temperature control chip comprises an upper chip 1 and a lower chip 2, wherein the upper chip 1 and the lower chip 2 are silicon substrates with insulating layers on both front and back surfaces.
The general structure of the silicon substrate is shown in fig. 1, and includes a substrate silicon 31 and insulating layers on both sides of the substrate silicon 31, wherein the insulating layer 32 may be a silicon nitride layer or a silicon oxide layer. In this embodiment, the thickness of the insulating layer is 20-300 nm, and the thickness of the silicon substrate is 50-500 μm.
Referring to fig. 2, the front surface of the upper sheet 1 and the front surface of the lower sheet 2 are fixedly bonded by an adhesive layer 4, and the upper sheet 1, the lower sheet 2 and the adhesive layer 4 together form a closed chamber 5. The adhesive layer 4 may be a glue capable of bonding and fixing the upper sheet 1 and the lower sheet 2, or may be a bonding metal layer directly fixing the upper sheet 1 and the lower sheet 2 by metal bonding. The height of the cavity 5 may be determined by the thickness of the adhesive layer 4, or may be determined by the heights of the bosses provided on the upper sheet 1 and the lower sheet 2 and the thickness of the adhesive layer 4.
Referring to fig. 2 and 3, the upper plate 1 is provided with a first window 11, and the first window 11 may be formed on the silicon substrate by etching, specifically, the insulating layer on the reverse side of the corresponding region and the substrate silicon are etched away by etching, and only the insulating layer on the front side of the corresponding region remains.
Referring to fig. 2 and 4, the lower sheet 2 is provided with a liquid injection port 21, an outlet port 22, a heating layer 23 and a second window 24, wherein the liquid injection port 21 and the outlet port 22 are communicated with the chamber 5, the liquid injection port 21 and the outlet port 22 can be realized by etching away the substrate silicon on the corresponding region and the insulating layers on the front and back sides of the corresponding region, and the second window 24 can be realized by etching away the insulating layer on the back side and the substrate silicon on the corresponding region and leaving only the insulating layer on the front side of the corresponding region.
The heating layer 23 further has a heating wire 25 located on the second window 24, and the heating wire 25 is in a spiral ring shape with a gap therebetween and is not connected to each other, and is disposed in the second window. The heating wire 25 is made of gold, platinum, palladium, rhodium, molybdenum, tungsten, platinum-rhodium alloy or nonmetal molybdenum carbide, and has a thickness of 30-100 nanometers; the area occupied by the heating wires is not more than a square area of three microns by three microns, and the gap between the heating wires is 20 to 200 nanometers.
The heating layer 23 further has four contact electrodes 231 extending to the edge of the lower sheet 2 and exposed, the four contact electrodes 231 form two pairs, one pair serves as a heating electrode, the other pair serves as a monitoring electrode, so that the heating layer is configured into two groups of equivalent circuits, and the two groups of equivalent circuits are respectively controlled by using a separate current source meter and a separate voltage source meter; one loop of the two equivalent circuits is responsible for power supply and heat production, the other loop is responsible for monitoring the resistance value of the heating wire after heating in real time, and the resistance of the test circuit is adjusted in real time through the feedback circuit according to the correlation between the resistance (R) and the temperature (T) in the design program so as to reach the set temperature.
When the upper sheet and the lower sheet are bonded and fixed, a special chip assembling instrument can be adopted for assembling, the first window 11 of the upper sheet 1 and the second window 24 of the lower sheet 2 are aligned, the observation windows are too small due to skew, the windows can not be found, and the electron beams cannot penetrate through the windows if the windows are not aligned.
The whole size of the heater strip of electron microscope fluid infinitesimal temperature control chip that this embodiment provided can reach about 1 micron at least, interval between the heater strip can reach 20 nanometers at least, thereby can direct observation heater strip appearance in the observation window, this micro-district heater strip has heating and accuse temperature dual function, can be used for real-time feedback fluid infinitesimal reaction temperature and provide the required temperature of reaction, the person of facilitating the use knows the chemical reaction of local position in the fluid solution better and inhales and release the heat reaction type, the temperature change between the fluid infinitesimal can directly perceived the acquisition to the reaction influence, and this electron microscope fluid infinitesimal temperature control chip still has fast rising and falling the temperature, accurate temperature control measurement, the resolution ratio is high, the advantage that the sample drift rate is low.
Example 2
The present embodiment also provides a method for manufacturing an electron microscope fluid micro element temperature control chip by using an ion beam, where the method can be used to manufacture the electron microscope fluid micro element temperature control chip described in embodiment 1.
The method comprises the following steps:
s1: processing a first window on a silicon substrate A with insulating layers on the front and back surfaces to manufacture an upper wafer;
s2: processing four contact electrodes, a liquid inlet, a liquid outlet, a second window and heating wires on a silicon substrate B with insulating layers on the front and back surfaces, wherein the heating wires are in a spiral ring shape which is provided with gaps and is not connected with each other and are arranged in the second window to manufacture a lower piece;
s3: and fixedly bonding the upper sheet and the lower sheet through the bonding layer, and aligning the centers of the first window and the second window to obtain the electron microscope fluid infinitesimal temperature control chip.
Preferably, step S2 includes:
s21: transferring the patterns of the second window, the liquid inlet and the liquid outlet from the photoetching mask plate to the back surface of the silicon substrate B with insulating layers on the front and back surfaces by adopting a photoetching process, developing in a positive photoresist developing solution, and washing with deionized water to obtain a silicon substrate B1;
s22: removing the insulating layer corresponding to the liquid inlet, the liquid outlet and the second window on the back surface of the silicon substrate B1 by adopting a reactive ion etching or ion beam etching process, and then removing the photoresist to obtain a silicon substrate B2;
s23: putting the silicon chip into a KOH solution or a tetramethylammonium hydroxide solution by adopting a wet etching process, removing the substrate silicon corresponding to the liquid inlet, the liquid outlet and the second window of the silicon chip B2, then, soaking and washing the silicon chip with an acid solution, and washing the silicon chip with deionized water to obtain a silicon chip B3;
s24: transferring the rectangular position patterns of the contact electrodes and the window predicted etching heating wires to the front surface of a silicon substrate B3 from a photoetching mask plate by adopting a laser direct-writing photoetching or ultraviolet photoetching process, developing in a positive photoresist developing solution, and washing with deionized water to obtain a silicon substrate B4;
s25: sputtering a heating material film on the front surface of a silicon substrate B4 by adopting a direct current magnetron sputtering, thermal evaporation coating or electron beam evaporation coating process, connecting electrodes through a square metal film with the diameter not more than 5 microns by 5 microns, soaking the electrodes in acetone to remove the photoresist and the metal film on the photoresist, washing the electrodes with deionized water, removing the photoresist, soaking the photoresist in acetone, and washing the electrodes with the deionized water to obtain a silicon substrate B5;
s26: carrying out laser scribing on the silicon substrate B5 to obtain a single chip B6;
s27: and removing redundant heating membrane filaments at the position of the heating filament on the single sheet B6 by adopting a focused ion beam ion etching process, and transferring the pattern of the heating filament to a window to obtain a lower sheet.
Preferably, the photolithography process used in step S21 is: and (3) exposing in a hard contact mode of an ultraviolet lithography machine, wherein the developing time is 45 seconds, and the exposing time is 10-30 seconds.
Preferably, the reactive ion etching process adopted in step S22 is: the etching rate is 10-20 nanometers per second, and the etching time is 10-120 seconds.
Preferably, the wet etching process adopted in step S23 is: and (3) etching by using a potassium hydroxide solution with the mass percentage concentration of 20-50%, wherein the etching temperature is 60-100 ℃, and the etching time is 2-4 hours.
Preferably, the photolithography process used in step S24 is: and (3) exposing in a hard contact mode of an ultraviolet lithography machine, wherein the developing time is 45 seconds, and the exposing time is 10-30 seconds.
Preferably, the coating process adopted in step S25 is: the vacuum degree reaches 7.6 x 10-5, a 3-10 nanometer titanium film is sputtered to serve as an adhesive layer, a 100-300 nanometer metal film is sputtered to serve as a heating wire, and the metal film can be made of materials such as platinum, molybdenum, tungsten, gold, semiconductors, piezoelectric ceramics and the like.
Preferably, step S27 includes: bombarding and etching with gallium ion beam at current of 10-20pA and residence time of 10-15 μ S, and repeating for 5-7 times.
While the invention has been particularly shown and described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. The utility model provides an electronic speculum fluid infinitesimal accuse temperature chip, includes upper segment and lower segment, and upper segment and lower segment all are the silicon substrate that the positive and negative all was equipped with the insulating layer, and the front of upper segment is fixed through the tie coat with the front of lower segment, and upper segment, lower segment and tie coat constitute an inclosed cavity jointly, are provided with first window on the upper segment, are equipped with on the lower segment and annotate liquid mouth, egress opening, zone of heating and second window, and first, second window is just to setting up its characterized in that: still be connected with the heater strip on the zone of heating, the heater strip is the spiral annular that leaves the clearance each other, interconnect, the heater strip is laid in the second window.
2. The electron microscope fluid micro element temperature control chip according to claim 1, characterized in that: the area occupied by the heating wires is not more than a square area with the length of three microns by three microns, the heating wires are positioned in the central area of the second window, and the gaps among the heating wires are 20-200 nanometers.
3. The electron microscope fluid micro element temperature control chip according to claim 1, characterized in that: the heating layer comprises four contact electrodes, and the four contact electrodes form two pairs, wherein one pair is used as a heating electrode, and the other pair is used as a monitoring electrode.
4. The electron microscope fluid micro element temperature control chip according to claim 1, characterized in that: the heating wire is manufactured by a material reducing process, the film material of the heating wire is subjected to film coating deposition in advance, and the heating wire is accurately cut into spiral rings which are mutually provided with gaps, uniform and unconnected by focused ion beams in a vacuum environment.
5. The electron microscope fluid micro element temperature control chip according to claim 1, characterized in that: the heating wire is made of platinum, molybdenum, tungsten, gold, semiconductor or piezoceramic materials.
6. A method for manufacturing an electron microscope fluid micro-element temperature control chip by ion beam etching is characterized by comprising the following steps:
s1, processing a first window on the silicon substrate A with the insulating layer on the front and back surfaces to manufacture an upper wafer;
s2, processing four contact electrodes, a liquid inlet, a liquid outlet, a second window and heating wires on a silicon substrate B with insulating layers on the front and back surfaces, wherein the heating wires are spiral rings which are not connected and have gaps, and are arranged in the second window to manufacture a lower piece;
and S3, fixing the upper plate and the lower plate under a chip assembling instrument through bonding layers, and aligning the centers of the first window and the second window to obtain the transmission electron microscope fluid temperature control infinitesimal temperature control chip.
7. The method according to claim 6, wherein step S2 includes:
s21, transferring the patterns of the second window, the liquid inlet and the liquid outlet from the photoetching mask plate to the back surface of the silicon substrate B with insulating layers on the front and back surfaces by adopting a photoetching process, developing in a positive photoresist developing solution, and washing with deionized water to obtain a silicon substrate B1;
s22, removing the insulating layer corresponding to the liquid inlet, the liquid outlet and the second window on the back of the silicon substrate B1 by adopting a reactive ion etching or ion beam etching process, and then soaking in an acetone solution to remove the photoresist to obtain a silicon substrate B2;
s23, putting the silicon wafer into a KOH solution or a tetramethylammonium hydroxide solution by adopting a wet etching process, removing the substrate silicon corresponding to the liquid inlet, the liquid outlet and the second window of the silicon substrate B2, then soaking and washing the silicon substrate B2 with an acid solution, and washing the silicon substrate with deionized water to obtain a silicon substrate B3;
s24, transferring the heating electrode and the rectangular position pattern with the predicted heating wire etched on the window from the photoetching mask plate to the front side of the silicon substrate B3 by adopting a laser direct-writing photoetching or ultraviolet photoetching process, developing in positive photoresist developing solution, and washing with deionized water to obtain a silicon substrate B4;
s25, adopting direct current magnetron sputtering coating, thermal evaporation coating and electron beam evaporation coating processes, sputtering a layer of heating material film on the front surface of the silicon substrate B4, soaking the silicon substrate B4 with acetone, washing the silicon substrate with deionized water, and removing photoresist to obtain a silicon substrate B5;
s26: carrying out laser scribing on the silicon substrate B5 to obtain a single chip B6;
s27: and removing redundant heating membrane filaments at the position of the heating filament on the single sheet B6 by adopting a focused ion beam ion etching process, and transferring the pattern of the heating filament to a window to obtain a lower sheet.
8. The method according to claim 7, wherein the photolithography process used in step S21 is: and (3) exposing in a hard contact mode of an ultraviolet lithography machine, wherein the developing time is 45 seconds, and the exposing time is 10-30 seconds. The reactive ion etching process adopted in step S22 is: the etching rate is 10-20 nanometers per second, and the etching time is 10-120 seconds. The wet etching process adopted in step S23 is: and (3) etching by using a potassium hydroxide solution with the mass percentage concentration of 20-50%, wherein the etching temperature is 60-100 ℃, and the etching time is 2-4 hours.
9. The method according to claim 7, wherein the photolithography process used in step S24 is: exposing in a hard contact mode of an ultraviolet lithography machine, wherein the developing time is 45 seconds, and the exposing time is 10-30 seconds; the coating process adopted in the step S25 is as follows: 3-10 nanometer titanium film is sputtered as an adhesive layer, and 100-300 nanometer metal film is sputtered as a heating wire.
10. The method of claim 7, wherein the focused ion beam etching process used in step S27 is: bombarding and etching with gallium ion beam at current of 10-20pA and residence time of 10-15 μ S, and repeating for 5-7 times.
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| CN101057309A (en) * | 2004-09-13 | 2007-10-17 | 代夫特工业大学 | Microreactor for a transmission electron microscope and heating element and method for the manufacture thereof |
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| CN111312573A (en) * | 2020-03-12 | 2020-06-19 | 厦门超新芯科技有限公司 | Transmission electron microscope high-resolution in-situ liquid phase heating chip and preparation method thereof |
| CN111354615A (en) * | 2020-03-12 | 2020-06-30 | 厦门超新芯科技有限公司 | Transmission electron microscope in-situ electro-thermal coupling chip and preparation method thereof |
| CN112516936A (en) * | 2020-12-18 | 2021-03-19 | 厦门大学 | Thermoelectric coupling micro flow reactor and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101057309A (en) * | 2004-09-13 | 2007-10-17 | 代夫特工业大学 | Microreactor for a transmission electron microscope and heating element and method for the manufacture thereof |
| CN109865541A (en) * | 2019-03-12 | 2019-06-11 | 厦门大学 | A kind of scanning electron microscope home position Electrochemical Detection chip and preparation method thereof |
| CN111312573A (en) * | 2020-03-12 | 2020-06-19 | 厦门超新芯科技有限公司 | Transmission electron microscope high-resolution in-situ liquid phase heating chip and preparation method thereof |
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