CN113990724B - Full two-dimensional vacuum tube and preparation method thereof - Google Patents
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- 239000000463 material Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000011810 insulating material Substances 0.000 claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- 238000005516 engineering process Methods 0.000 claims abstract description 6
- 239000002243 precursor Substances 0.000 claims abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 21
- 229910052582 BN Inorganic materials 0.000 claims description 20
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 20
- 238000000137 annealing Methods 0.000 claims description 19
- 229920000642 polymer Polymers 0.000 claims description 13
- 229910002804 graphite Inorganic materials 0.000 claims description 11
- 239000010439 graphite Substances 0.000 claims description 11
- 239000002998 adhesive polymer Substances 0.000 claims description 9
- 229910021389 graphene Inorganic materials 0.000 claims description 9
- 238000010894 electron beam technology Methods 0.000 claims description 6
- 238000005530 etching Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 4
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 4
- 239000012212 insulator Substances 0.000 claims description 4
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims description 4
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims description 4
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- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 4
- ROUIDRHELGULJS-UHFFFAOYSA-N bis(selanylidene)tungsten Chemical compound [Se]=[W]=[Se] ROUIDRHELGULJS-UHFFFAOYSA-N 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 3
- 238000012546 transfer Methods 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 238000005566 electron beam evaporation Methods 0.000 claims description 2
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- 230000004927 fusion Effects 0.000 claims description 2
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J21/00—Vacuum tubes
- H01J21/02—Tubes with a single discharge path
- H01J21/06—Tubes with a single discharge path having electrostatic control means only
- H01J21/10—Tubes with a single discharge path having electrostatic control means only with one or more immovable internal control electrodes, e.g. triode, pentode, octode
- H01J21/105—Tubes with a single discharge path having electrostatic control means only with one or more immovable internal control electrodes, e.g. triode, pentode, octode with microengineered cathode and control electrodes, e.g. Spindt-type
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y10/00—Nanotechnology for information processing, storage or transmission, e.g. quantum computing or single electron logic
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
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Abstract
The invention discloses a full two-dimensional vacuum tube and a preparation method thereof, and belongs to the technical field of nano materials. The invention combines the traditional vacuum tube technology with the modern transistor technology, and takes the two-dimensional insulating material as the precursor material of the vacuum channel in the vacuum tube; a two-dimensional conductive material transistor is used as a thermal field emission source-cathode; the metal conductive material is used as an electron collecting electrode-anode, the full two-dimensional vacuum tube is formed by vertically stacking full two-dimensional materials, and electrons are emitted by a thermal field between a cathode and an anode at two ends of a nano-scale vacuum channel of the full two-dimensional vacuum tube to form a basic electric behavior similar to diode unidirectional channel connection. The full two-dimensional vacuum tube can be prepared in an array manner, and is beneficial to being integrated into a modularized circuit. The method is applied to product platforms such as high-precision vacuum pressure sensors, new material NEMS micro-motor systems, radiation-resistant thermal field emission power transistors and the like.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a full two-dimensional vacuum tube and a preparation method thereof.
Background
The invention relates to a vacuum tube (also known as an electron tube, a liner, an English name vacuum tube, an electron tube, a valve and the like) which is an electronic component relying on thermionic emission, and the invention of the vacuum tube is mainly inspired by the research of the electron emission capability of a heating filament by Thomas and Edison. Prior to the advent of semiconductor transistors, they were used primarily in microelectronic and high power electronic circuits such as electronic circuits, glow displays, X-ray generators, microwave oscillators, and the like. The first electron tube computer end is composed of nearly twenty thousands of electron tubes. However, with the advent of solid state semiconductors, vacuum tubes have fallen behind in terms of miniaturization, low power consumption, etc., and the history stage of integrated circuits has gradually faded out in the fifth sixty of the last century.
Although vacuum tubes fail to show great significance in integrated circuits, transistors are not perfect. First, with the continuous shrinkage of transistor dimensions in recent 40 years, the gate dielectric layer of the MOSFET is only a few nanometers thick, and the channel length between the source and drain is also only tens of nanometers wide. Nevertheless, the pursuit of faster, more energy efficient chips continues, and it is apparent that typical MOSFETs have gradually failed to meet the demands of modern technological development; second, transistors are far inferior to vacuum tubes for transporting electronic media. Electrons are transmitted in vacuum without any scattering, and the transmission speed can be maximally close to the light speed of 3 multiplied by 10 10 cm/s, while in solid semiconductors electrons collide with atoms constantly, resulting in lattice scattering etc. at a transmission rate of up to 5X 10 7 cm/s, the carrier transport characteristics of the vacuum tube are therefore extremely advantageous. In addition, solid-state semiconductor devices are more susceptible to strong radiation than vacuum tubes, which can destroy the atomic structure of silicon, thereby preventing the correct movement of charges. This is a major problem for both military and aerospace institutions, which require their own equipment to function properly in highly radiating environments (e.g., outer space).
The current vacuum tube device generally still faces the problems of large mass and volume, high power consumption, difficult integration and the like. One solution to these problems is to micro-nano the vacuum tube to produce an on-chip vacuum electronic device. Research group of NASA in the united states space agency has demonstrated integrable micro-nano vacuum tubes using Si circuitry [ Nature Electronics,2,405,2019]The method comprises the steps of carrying out a first treatment on the surface of the The graphene and the carbon nano tube are suspended by Beijing university team in China, and the electron probe of a scanning electron microscope is adopted to study the thermal field emission effect in vacuum, and the current density can reach 1.33A/cm at maximum 2 [Nature Communications,7,11513,2015；Advanced Functional Materials,30,1907814,2020]。
However, to date, the study of full two-dimensional van der Waals vacuum tubes has remained blank. The full two-dimensional vacuum tube not only can further improve the performances of the device, such as the integration level, the measurable quantity and the like, but also has great application potential in the aspects of power devices, lab-on-a-chips (lab-on-a-chips), and the like; the following characteristics are also provided: the excellent radiation immunity characteristic enables the radiation immune type fluorescent dye to be directly applied to extreme environments such as aerospace, nuclear radiation and the like; (II) extremely fast response speed, making it a so-called high frequency technology candidate; and (III) it is used as a miniature X-ray tube for detecting the "fingerprint" of certain fixed frequency molecules.
Disclosure of Invention
Aiming at the problems of large quality and volume, high power consumption and difficult integration of the existing vacuum tube device, the invention provides a full two-dimensional vacuum tube and a preparation method thereof.
The invention discloses a method for realizing a novel full-two-dimensional vacuum tube with a vacuum channel and a compatible MOSFET (Metal-oxide-semiconductor field Effect transistor) framework. The invention adopts two-dimensional layered materials as the joule heat emission material and the vacuum channel, overcomes the mass and size limitation of the traditional vacuum tube, greatly reduces the size and the mass of the device, and provides a precursor nanostructure for labs on chip, power devices, nano score point systems, micro-nano X-ray tubes and the like.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the full two-dimensional vacuum tube is prepared by taking a two-dimensional insulating material as a precursor material of a vacuum channel in the vacuum tube; a two-dimensional conductive material transistor is used as a thermal field emission source-cathode; the metal conductive material is used as an electron collecting electrode-anode.
Further, the two-dimensional insulating material is a two-dimensional layered material with good dielectric properties; the metal conductive material is any one of graphite and Au, pd, ti, ni; the two-dimensional conductive material is a material with good joule heat emission performance. The two-dimensional insulating material prevents dielectric breakdown phenomenon from occurring and influences the performance of the vacuum tube; a metal conductive material for securing stability of an anode voltage; a two-dimensional conductive material for providing a stable thermal field emission current.
Further, the two-dimensional insulating material is hexagonal boron nitride with the thickness of 200-400 nm and MnPSe 3 。
Further, the two-dimensional conductive material is any one of graphene, few-layer graphene, thin-layer graphite, molybdenum disulfide and tungsten diselenide. At present, experiments prove that the materials have good Joule heat emission performance and can bear ultrahigh current density.
The preparation method of the full two-dimensional vacuum tube comprises the following steps:
step 1, carrying out hole etching treatment on a two-dimensional insulating material by adopting an electron beam exposure and etching technology to prepare a vacuum channel in a vacuum tube so as to obtain a hole insulator;
step 2, using adhesive polymer to transfer the hole insulator of the vacuum channel in the step 1 to the surface of the metal conductive material to form a double-layer structure, and volatilizing all the residual polymer on the surface to obtain a clean surface;
step 3, transferring the boron nitride and the two-dimensional conductive material to the surface of the double-layer structure in the step 2 by using a viscous polymer, and slowly heating to 160 ℃ for fusion to obtain a four-layer stacking heterostructure;
step 4, volatilizing all the surface residual polymer in the step 3, and evaporating a metal electrode through electron beam exposure and electron beam evaporation;
and 5, performing patterning treatment through electron beam exposure and reactive ion etching to obtain an electron emission electrode-cathode in the vacuum tube, and completing the preparation of the full two-dimensional vacuum tube.
Further, the insulating material is hexagonal boron nitride with the thickness of 200-400 nm and MnPSe 3 。
Further, the adhesive polymer is an arc-shaped PDMS/PPC double-layer structure material. The PDMS is an arc-shaped substrate naturally dried in a liquid drop mode, and the adhesive polymer can completely transfer the two-dimensional material.
Further, the two-dimensional conductive material is any one of graphene, few-layer graphene, thin-layer graphite, molybdenum disulfide and tungsten diselenide.
Further, the surface residual polymer was totally volatilized by the annealing treatment. Compared with the method of cleaning with acetone, the method does not damage the sample and pollute the surface, and the surface after treatment is cleaner.
Further, the annealing treatment is vacuum annealing or inert gasAny one of atmosphere annealing; the vacuum degree of the vacuum annealing is not lower than 10 -3 mbar; the inert atmosphere in the inert atmosphere annealing is argon and argon-hydrogen mixed gas; the vacuum degree is not lower than 10mbar. Preventing degradation of the sample at high temperatures, or surface modification. The annealing temperature of the annealing treatment is not lower than 100 ℃. Ensure that the polymer on the surface of the sample can be totally volatilized.
Compared with the prior art, the invention has the following advantages:
1. cheng Jianrong to solid state electronic devices of currently mainstream semiconductors (silicon, etc.);
2. the novel full-two-dimensional vacuum tube with a vacuum channel and a compatible MOSFET architecture can be realized on the basis of being compatible with the process of the solid-state electronic device of the current mainstream semiconductor (silicon and the like), and the vertical dimension is reduced to 200nm;
3. the full two-dimensional vacuum tube can be prepared in an array manner, and is beneficial to being integrated into a modularized circuit. The method is applied to product platforms such as high-precision vacuum pressure sensors, new material NEMS micro-motor systems, radiation-resistant thermal field emission power transistors and the like.
Drawings
FIG. 1 is a schematic diagram of an overall two-dimensional vacuum tube structure according to the present invention;
FIG. 2 is a schematic diagram of the overall two-dimensional vacuum tube manufacturing process of the present invention;
FIG. 3 is a schematic diagram of an overall two-dimensional vacuum tube device according to example 1;
fig. 4 is a schematic diagram of an all two-dimensional vacuum tube device in example 2.
Detailed Description
Example 1
An all-dimensional vacuum tube device using 300nm hole boron nitride as a vacuum channel, 13.5nm graphite as a vacuum tube cathode, and an Au/Ti (30/5 nm) electrode as a vacuum tube anode is shown in FIG. 3.
As shown in the flow chart of FIG. 2, hexagonal boron nitride with the thickness of about 300nm is etched by adopting a reactive ion etching technology to form holes with the size of 1 multiplied by 4 mu m 2 Then transferring the polymer to the surface of Au/Ti (30/5 nm) electrode to form a boron nitride/Au electrode double-layer structure, and carrying out vacuum annealingFire treatment; transferring the boron nitride/graphite double-layer structure transferred to the surface of the adhesive polymer to the surface of the hole boron nitride, and removing the residual polymer on the surface of the hole boron nitride by high vacuum annealing to form a four-layer stacking heterostructure; and then carrying out the vapor deposition of the electrode and the patterning treatment of the thermal emission area to prepare the novel full-two-dimensional vacuum tube device with a vacuum channel and compatible with the MOSFET architecture.
Wherein fig. 3a is an optical photograph of the device, the black dotted line area is the anodic Au electrode area, and the scale is 10 μm.
As shown in fig. 3b, which is an SEM scan of a device with a scale of 1 μm, it can be seen by SEM scanning that the cathode electrode in the device is not collapsed, damaged, and suspended well above the hole.
FIG. 3c is a graph showing the thermal field emission curve of the anode V, as measured by thermal field emission c When the voltage is=45v, the emission current can reach 10nA, and the on-state voltage V on 1V, see FIG. 3c, with the inset being an enlarged view.
Example 2
A full two-dimensional vacuum tube device with 200nm hole boron nitride as a vacuum channel, single-layer graphene as a vacuum tube cathode and a graphite electrode as a vacuum tube anode;
etching hexagonal boron nitride with thickness of about 200nm by reactive ion etching to obtain a hole with size of 3×3μm 2 Obtaining hole boron nitride, transferring the hole boron nitride to the surface of metal graphite by using an adhesive polymer to form a boron nitride/graphite double-layer structure, and removing the residual polymer on the surface by vacuum annealing treatment to obtain a clean surface; transferring the boron nitride/single-layer graphene double-layer structure transferred to the surface of the adhesive polymer to the surface of the hole boron nitride, and removing the residual polymer on the surface of the hole boron nitride by high vacuum annealing to form a four-layer stacking heterostructure; and then carrying out the vapor deposition of the electrode and the patterning treatment of the thermal emission area to prepare the novel full-two-dimensional vacuum tube device with a vacuum channel and compatible with the MOSFET architecture.
Wherein fig. 4a is an optical photograph of the device, the black dotted line area is the anode graphite area, and the scale is 10 μm.
As shown in FIG. 4b, the thermal field emission curve is shown, and it is found by thermal field emission measurement that when the anode V c When the current is=40v, the emission current can reach 160pA, and the inset is a partial enlarged image.
The present invention uses a PDMS/PPC bilayer adhesive polymer, unless otherwise specified.
What is not described in detail in the present specification belongs to the prior art known to those skilled in the art. While the foregoing describes illustrative embodiments of the present invention to facilitate an understanding of the present invention by those skilled in the art, it should be understood that the present invention is not limited to the scope of the embodiments, but is to be construed as protected by the accompanying claims insofar as various changes are within the spirit and scope of the present invention as defined and defined by the appended claims.
Claims (8)
1. A preparation method of a full two-dimensional vacuum tube is characterized by comprising the following steps: the method comprises the following steps:
step 1, carrying out hole etching treatment on a two-dimensional insulating material by adopting an electron beam exposure and etching technology to prepare a vacuum channel in a vacuum tube so as to obtain a hole insulator;
step 2, using adhesive polymer to transfer the hole insulator of the vacuum channel in the step 1 to the surface of the metal conductive material to form a double-layer structure, and volatilizing all the residual polymer on the surface to obtain a clean surface;
step 3, transferring the boron nitride and the two-dimensional conductive material to the surface of the double-layer structure in the step 2 by using a viscous polymer, and slowly heating to 160 ℃ for fusion to obtain a four-layer stacking heterostructure;
step 4, volatilizing all the surface residual polymer in the step 3, and evaporating a metal electrode through electron beam exposure and electron beam evaporation;
step 5, carrying out graphic processing through electron beam exposure and reactive ion etching to obtain an electron emission electrode-cathode in the vacuum tube, and completing the preparation of the full two-dimensional vacuum tube;
the two-dimensional conductive material is any one of graphene, few-layer graphene, thin-layer graphite, molybdenum disulfide and tungsten diselenide.
2. The method for manufacturing the full two-dimensional vacuum tube according to claim 1, wherein the method comprises the following steps: the two-dimensional insulating material is hexagonal boron nitride with the thickness of 200-400 nm and MnPSe 3 。
3. The method for manufacturing the full two-dimensional vacuum tube according to claim 1, wherein the method comprises the following steps: the adhesive polymer is an arc PDMS/PPC double-layer structure material.
4. The method for manufacturing the full two-dimensional vacuum tube according to claim 1, wherein the method comprises the following steps: the surface residual polymer was totally volatilized by annealing treatment.
5. The method for manufacturing a full two-dimensional vacuum tube according to claim 4, wherein: the annealing treatment is any one of vacuum annealing and inert atmosphere annealing; the vacuum degree of the vacuum annealing is not lower than 10 -3 mbar; the inert atmosphere in the inert atmosphere annealing is argon and argon-hydrogen mixed gas; vacuum degree is not lower than 10mbar; the annealing temperature of the annealing treatment is not lower than 100 ℃.
6. An all-two-dimensional vacuum tube made by the method of claim 5, wherein: the full two-dimensional vacuum tube is made of a two-dimensional insulating material serving as a precursor material of a vacuum channel in the vacuum tube; a two-dimensional conductive material transistor is used as a thermal field emission source-cathode; the metal conductive material is used as an electron collecting electrode-anode.
7. A full two-dimensional vacuum tube as defined in claim 6, wherein: the two-dimensional insulating material is a two-dimensional layered material with good dielectric properties; the metal conductive material is any one of graphite and Au, pd, ti, ni; the two-dimensional conductive material is a material with good joule heat emission performance.
8. A full two-dimensional vacuum tube as defined in claim 6, wherein: the two-dimensional insulating material is hexagonal boron nitride with the thickness of 200-400 nm and MnPSe 3 。
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