CN109904052B - Ion neutralizer device and preparation method thereof - Google Patents
Ion neutralizer device and preparation method thereof Download PDFInfo
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- CN109904052B CN109904052B CN201811654080.7A CN201811654080A CN109904052B CN 109904052 B CN109904052 B CN 109904052B CN 201811654080 A CN201811654080 A CN 201811654080A CN 109904052 B CN109904052 B CN 109904052B
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Abstract
The invention discloses an ion neutralizer device and a preparation method thereof, wherein the ion neutralizer device comprises the following steps: the device comprises a cathode substrate, a carbon nanotube array, metal nanoparticles, an insulating layer and a metal grid electrode; the carbon nano tube array is deposited on a cathode substrate, the metal nano particles are dispersed on the carbon nano tube array, and the carbon nano tube array is uniformly modified to form a carbon nano tube array cathode; the insulating layer is positioned on the surface of the cathode substrate, the insulating layer is hollow, and the carbon nanotube array cathode is positioned in the hollow part of the insulating layer; the metal grid electrode is of a hollow structure, the array of the carbon nano tubes is aligned with the hollow position of the metal grid electrode to form a sandwich structure, and the array cathode of the carbon nano tubes, the metal grid electrode and the insulating layer are ensured not to be conducted with each other. The invention reduces the contact resistance between the carbon nano tube and the substrate, reduces the heat effect of the device and the whole power consumption, and improves the service life and the reliability of the neutralizer.
Description
Technical Field
The invention relates to the crossing field of vacuum microelectronic technology and micro-nano processing preparation, in particular to an ion neutralizer device and a preparation method thereof.
Background
Electric propulsion systems have developed over the years as key devices in the field of space applications. In order to meet the high-difficulty space detection tasks borne by various detection satellites at present, the method has great significance for improving the control precision of the satellite orbit and attitude. Therefore, the development of an electric propulsion system capable of providing milli-Newton (or micro-Newton) thrust and having high-precision thrust control performance is a key technical means for solving the problems of high-precision attitude and orbit adjustment in the aerospace scientific probe at present. The electric propulsion system is mainly composed of three structures: ionization systems, ion acceleration systems, and ion neutralization systems. The ion neutralizing system has the main function of emitting electrons to neutralize positively charged ions ejected from the propulsion system, so as to prevent a large amount of positively charged ions from accumulating in the electric propulsion system and affecting the service life of the system.
In the working mechanism of the existing field emission cathode ion neutralizer, high voltage driving is a necessary working condition for generating electron current. However, relevant researches show that the high-voltage electric field has obvious influence on the structural stability of the one-dimensional carbon nanotube. First, since the diameter of the carbon nanotube is small, the uniformity and consistency of the grown carbon tube are difficult to ensure, and therefore, the tip passivation phenomenon, also known as the field shielding phenomenon, occurs on a part of the tip carbon tubes due to high emission utilization rate, which may cause the stability of the entire emission array to be affected. Secondly, the contact between the carbon tube and the surface of the substrate is not good ohmic contact generally, a Schottky barrier exists, and obvious thermal effect can occur in long-time work to damage the structure of the carbon tube and cause short circuit, thereby influencing the reliability of the ion neutralizer. Generally, the lifetime of a space-cathode tube can be more than 50000 hours, while the working limit of a field emission cathode tube is generally about 5000 hours because of the above two effects. How to improve the reliability and the service life of the carbon nanotube field emission ion neutralizer is a critical problem which needs to be solved at present.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to solve the technical problems of short service life and poor stability of the existing carbon nanotube field emission ion neutralizer.
To achieve the above object, in a first aspect, the present invention provides an ion neutralizer device comprising: the device comprises a cathode substrate, a carbon nanotube array, metal nanoparticles, an insulating layer and a metal grid electrode;
the carbon nano tube array is deposited on a cathode substrate, the metal nano particles are dispersed on the carbon nano tube array, and the carbon nano tube array is uniformly modified to form a carbon nano tube array cathode;
the insulating layer is positioned on the surface of the cathode substrate, the insulating layer is hollow, and the carbon nanotube array cathode is positioned in the hollow part of the insulating layer;
the metal grid electrode is of a hollow structure, the array of the carbon nano tubes is aligned with the hollow position of the metal grid electrode to form a sandwich structure, and the array cathode of the carbon nano tubes, the metal grid electrode and the insulating layer are ensured not to be conducted with each other.
Specifically, the carbon nanotube array and the carbon nanotube array cathode in the present invention essentially refer to a concept that the carbon nanotube array serves as a cathode of the ion neutralizer device. Further, the metal mesh electrode serves as an anode of the ion neutralizer device.
Optionally, the insulating layer is connected with the cathode substrate and the metal grid electrode in a bonding manner.
Optionally, the metal nanoparticles are obtained by depositing a metal thin layer on the surface of the nanotube array and annealing the metal thin layer.
In a second aspect, the present invention provides a method of making an ion neutralizer device, comprising the steps of:
(1) sequentially manufacturing a graphical buffer layer and a graphical catalyst layer on the surface of a cathode substrate from bottom to top, and growing a carbon nanotube array on the catalyst layer by a thermal chemical vapor deposition method;
(2) depositing a metal thin layer on the surface of the carbon nano tube array by adopting atomic layer deposition, and forming uniformly dispersed metal nano particles on the surface of the carbon nano tube array through annealing treatment to obtain a carbon nano tube array cathode uniformly modified by the metal nano particles;
(3) manufacturing a hollowed-out grid structure by a photoetching process, and depositing a uniformly-coated conducting layer on the surface of the hollowed-out grid structure by adopting atomic layer deposition to obtain a metal grid electrode;
(4) the carbon nanotube array cathode and the metal grid electrode are packaged through an insulating layer, the insulating layer is located on the surface of the cathode substrate, the insulating layer is hollow, the carbon nanotube array cathode uniformly modified by metal nanoparticles is located in the hollow part of the insulating layer, the array of the carbon nanotubes is aligned with the hollowed-out position of the grid structure to form a sandwich structure, and the array cathode of the carbon nanotubes, the metal grid electrode and the insulating layer are ensured not to be conducted with each other.
Optionally, the step (4) specifically includes the following steps:
respectively cutting the carbon nanotube array cathode, the insulating layer and the metal grid electrode to obtain a discrete carbon nanotube array cathode unit, and the insulating layer and the metal grid electrode which correspond to the discrete carbon nanotube array cathode unit;
the carbon nanotube array cathode unit and the insulating layer are connected in an aligning way to ensure that the carbon nanotube array cathode unit and the insulating layer are not conducted;
and connecting the metal grid electrode with the insulating layer connected with the carbon nanotube array cathode unit to ensure that the array cathode unit of the carbon nanotube is aligned with the hollow position of the grid structure.
Optionally, the step (4) specifically includes the following steps:
aligning the cathode of the carbon nanotube array and the insulating layer, and connecting the cathode of the carbon nanotube array and the insulating layer in a wafer bonding mode to ensure that the cathode of the carbon nanotube array and the insulating layer are not conducted;
connecting a metal grid electrode with an insulating layer connected with a carbon nanotube array cathode in a wafer bonding mode, and ensuring that an array cathode unit of a carbon nanotube is aligned with a hollow-out position of a grid structure to form a sandwich structure;
and cutting the wafer to obtain the discrete ion neutralizer.
Optionally, before the patterned buffer layer and the catalytic layer are sequentially formed on the surface of the cathode substrate from bottom to top, the cathode substrate is subjected to cleaning pretreatment.
Optionally, before the hollowed-out grid structure is manufactured by the photolithography process, the grid substrate is subjected to cleaning pretreatment.
Generally, compared with the prior art, the above technical solution conceived by the present invention has the following beneficial effects:
the metal nanoparticle modified carbon nanotube field emission neutralizer provided by the invention has the advantages of miniaturization, low power consumption, no fuel and the like, and is very suitable for being applied to a micro-Newton electric propulsion system. The uniform modification of the metal nano particles can reduce the working voltage of the neutralizer, improve the emission efficiency and reduce the contact resistance between the carbon nano tube and the substrate, thereby reducing the heat effect and the overall power consumption of the device and improving the service life and the reliability of the neutralizer.
According to the invention, due to the adoption of the atomic layer deposition technology, the nano film can be uniformly deposited on the surface and the bottom of the carbon nano tube array, and the phenomenon that the metal deposition process is not uniform and a field shielding effect occurs due to the influence of the size is avoided. The atomic layer deposition technology can be applied to a wide range of materials, the thickness of a deposited film can be accurately controlled to be atomic size, the manufacturing process of the neutralizer emitter has universality, and the type and size of modified metal particles can be regulated and controlled.
Drawings
FIG. 1 is a schematic view of the overall structure of an ion neutralizer according to the present invention;
FIG. 2a is a cross-sectional view of a cathode substrate structure of an emitter provided by the present invention, wherein 101 is a cathode substrate;
fig. 2b is a schematic diagram of a patterned carbon nanotube array fabricated on a cathode substrate of an emitter according to the present invention, where 201 is a carbon nanotube array;
FIG. 2c is a schematic diagram of an emitter after growing a metal thin layer by atomic layer deposition, where 202 is the metal thin layer;
fig. 2d is a schematic diagram of the emitter of the uniformly coated metal nanoparticles obtained by annealing treatment according to the present invention, and 203 is the metal nanoparticles;
fig. 2e is a schematic diagram of the present invention after the insulating layer and the cathode substrate are packaged, wherein 301 is the insulating layer;
fig. 2f is a schematic diagram of the metal grid electrode structure provided by the present invention after being aligned and encapsulated with the insulating layer and the cathode substrate, and 401 is a metal grid electrode;
FIG. 3a is a top view of a diced cathode emitter chip unit provided by the present invention;
FIG. 3b is a top view of a cut metal grid electrode chip unit according to the present invention;
FIG. 3c is a top view of a cell of an ion neutralizer device according to the present invention;
FIG. 4a is a schematic diagram of surface field emission of a carbon nanotube cathode without metal nanoparticle modification in a high vacuum and high pressure environment;
FIG. 4b is a schematic diagram of the surface field emission of the carbon nanotube cathode modified by the metal nanoparticles in a high vacuum and high pressure environment according to the present invention;
FIG. 5a is a schematic diagram of the electron emission performance of the cathode surface of the carbon nanotube modified by the metal nanoparticles in the high vacuum and high pressure environment according to the present invention;
fig. 5b is a schematic diagram of electron transport between the cathode of the carbon nanotube modified by the metal nanoparticles and the surface of the substrate in a high vacuum and high pressure environment according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The selection of the emitter nano material in the existing field emission ion neutralizer is also very wide, and structurally, the field emission ion neutralizer comprises nano particles, nano wires, nano tubes, nano sheets, three-dimensional nano nets and the like. Among them, the one-dimensional structure nano material is the most mature material and generally accepted in the industry, and due to the special tip morphology, under the bias of an applied voltage, a local electric field enhancement is formed, so that the electron emission efficiency of the emitter can be remarkably improved. In addition to the morphological structure, there have been numerous studies on the selection of materials, metallic materials, metal oxides and transition metal halides, etc., which are used in the manufacture of electron emitters. The results show that the vertical one-dimensional carbon nanotube array has the most ideal application prospect in the cathode emitter materials because of the excellent structure and material stability, is less affected under the high-pressure or high-temperature environment, and compared with other metal compounds, the conductivity of the multi-wall carbon nanotube has several orders of magnitude advantages, and is close to the metal materials. Carbon nanotube arrays are also few that have been practically used in electric thruster ion neutralizers, where the Lisa pathfinder distribution Reduction System (ST7-DRS) System employs a field emission ion neutralizer based on carbon nanotube arrays.
At present, the development of the commercial cathode neutralizer developed aiming at the micro-Newton electric propulsion system is slow in China. Unlike the traditional hollow cathode neutralizer applied to the common electric propulsion system, the emission efficiency of the cathode neutralizer is only a consideration in order to meet the requirements of high-precision and micro-Newton-level thrust regulation. In addition, low power consumption, small driving voltage, precisely adjustable output current and miniaturized device structure design are performance indexes to be met. The cathode neutralizer manufactured based on the carbon nanotube array field emission effect can emit instantly at normal temperature, realizes high emission efficiency and long reliability under low-voltage driving, and is an ion neutralizer most suitable for miniaturization and micro-Newton electric propulsion systems at present.
The invention provides a manufacturing scheme of an ion neutralizer suitable for a micro-Newton electric propulsion system. The scheme mainly adopts a one-dimensional vertical carbon nanotube array uniformly modified by metal nanoparticles as a cold cathode emitter, and then utilizes bonding or other packaging technologies to assemble the miniature ion neutralizer together with an insulating layer and a metal grid mesh electrode in a sandwich structure. The fabrication techniques rely primarily on semiconductor processing techniques. The metal nano-particles are modified by adopting a unique atomic layer deposition technology and a high-temperature annealing mode, so that the metal nano-particles can be uniformly coated on the compact vertical carbon nano-tube array.
The emitter manufacturing technical means of the invention all depend on the semiconductor micro-nano processing technology, and the distribution pattern of each emitter can be accurately adjusted. Secondly, the atomic layer deposition technology can not only uniformly coat the surface of the carbon nano tube, but also accurately regulate and control the thickness of the metal thin layer coated on the surface. Finally, the proper annealing temperature and time can be selected according to the metal characteristics, so that the surface metal thin layers are agglomerated to form nano-particles with similar dimensions. Because the atomic layer deposition technology can deposit a variety of metal materials, the thickness of the deposit can be accurately controlled to an atomic level, and the average size of the nanoparticles can be effectively controlled by changing the thickness of the metal film. Therefore, the method has universal applicability and good controllability for the modification of the surface nanoparticles of the carbon nanotubes.
Fig. 1 is a schematic view of an overall structure of an ion neutralizer provided in the present invention, as shown in fig. 1, including: a cathode substrate 101, a carbon nanotube array 201, metal nanoparticles 203, an insulating layer 301, and a metal grid electrode 401.
The carbon nanotube array 201 is deposited on the cathode substrate 101, the metal nanoparticles 203 are dispersed on the carbon nanotube array 201, and the carbon nanotube array 201 is uniformly modified to become a cathode of the carbon nanotube array 201; the insulating layer 301 is positioned on the surface of the cathode substrate 101, the insulating layer 301 is hollow, and the cathode of the carbon nanotube array 201 is positioned in the hollow part of the insulating layer 301; the metal grid electrode 401 is a hollow structure, the hollow positions of the array 201 of the carbon nanotubes and the metal grid electrode 401 are aligned to form a sandwich structure, and the cathode of the array 201 of the carbon nanotubes, the metal grid electrode 401 and the insulating layer 301 are ensured not to be conducted with each other.
Alternatively, the insulating layer 301 is connected to the cathode substrate 101 and the metal grid electrode 401 by bonding.
Alternatively, the metal nanoparticles 203 are obtained by depositing the metal thin layer 202 on the surface of the nanotube array 201, and annealing the metal thin layer 202.
The invention mainly utilizes a semiconductor micro-nano processing technology to manufacture a cathode neutralizer suitable for a micro-Newton level electric propulsion system. The emitter is manufactured by firstly patterning a cathode substrate and then adopting a vertical carbon nano tube array modified by metal nano particles. The metal grid electrode adopts a photoetching process to manufacture an array type hollow structure, and then the metal grid electrode is coated with a conducting layer through atomic layer deposition to manufacture an anode. The single emitter unit comprises a cathode with a carbon nanotube array, an insulating layer arranged on the edge of the cathode and a metal grid electrode on the top in sequence from bottom to top. The specific preparation process is as follows:
(1) as shown in fig. 2a, a cathode substrate 101 of an emitter is pretreated by cleaning and the like, a patterned buffer layer and a patterned catalytic layer are manufactured on the surface of the cathode substrate 101 through a photolithography process and material deposition, the buffer layer and the catalytic layer are sequentially arranged on the surface of the cathode substrate 101 from bottom to top, and as shown in fig. 2b, a carbon nanotube array 201 is grown on the surface of the cathode substrate 101 through a thermal chemical vapor deposition method;
(2) as shown in fig. 2c, depositing a metal thin layer 202 on the surface of the carbon nanotube array by atomic layer deposition, and performing annealing treatment at a proper temperature and time to form metal nanoparticles 203 on the surface of the carbon nanotube array, as shown in fig. 2d, to obtain a carbon nanotube array cathode uniformly modified by the metal nanoparticles;
as shown in fig. 2e, the insulating layer 301 is located on the surface of the cathode substrate 101, and the carbon nanotube array 201 is located in the hollow insulating layer.
(3) As shown in fig. 2f, the grid substrate is pretreated by cleaning, etc., a hollowed-out grid structure is manufactured by a photolithography process, and a uniformly coated conductive layer is deposited on the surface of the grid by atomic layer deposition to obtain a metal grid electrode 401;
(4) as shown in fig. 3a, 3b, 3c, there are two ways of device packaging, the first way: and respectively cutting the carbon nanotube cathode, the insulating layer and the metal grid electrode to obtain a discrete carbon nanotube cathode unit, and the insulating layer 301 and the metal grid electrode 401 corresponding to the discrete carbon nanotube cathode unit. Firstly, the carbon nanotube cathode unit and the insulating layer 301 are aligned and connected in bonding and other modes to ensure that the carbon nanotube cathode unit and the insulating layer 301 are not conducted, then the metal grid electrode 401 is connected with the insulating layer 301 connected with the carbon nanotube cathode unit in bonding and other modes to ensure that the array of the carbon nanotubes is aligned with the hollow structure of the grid, and finally a sandwich structure is formed and the three are not conducted. The second mode is as follows: firstly, the carbon nanotube cathode array 201 and the insulating layer 301 are aligned and connected in a wafer bonding mode to ensure that the carbon nanotube cathode array 201 and the insulating layer 301 are not conducted, and then the metal grid electrode 401 is connected with the insulating layer 301 connected with the carbon nanotube cathode unit in a wafer bonding mode to ensure that the carbon nanotube array is aligned with the hollow structure of the grid, and finally a sandwich structure is formed and the three are not conducted. And then cutting the wafer to obtain the discrete independent chip devices.
Aiming at the problems of short service life and poor stability of the carbon nanotube ion neutralizer, the invention provides a method for modifying metal nanoparticles of the carbon nanotube to improve the working performance of the neutralizer. The improvement of three aspects of the field emission property of the carbon nanotube array is mainly realized:
(1) as shown in fig. 4b, metal nanoparticles are uniformly distributed on the surface of the carbon nanotube, and amorphous carbon and surface impurities on the surface of the carbon nanotube are absorbed by the metal nanoparticles during the high-temperature annealing process, so that the work function of the emitter is reduced, and the emission efficiency is improved.
(2) As shown in fig. 5a, after the carbon nanotube surface is coated with the uniformly distributed metal nanoparticles, more electron emitter sites can be provided, so that the overall electron emission uniformity of the cathode emitter surface is improved, and the field shielding effect is reduced.
(3) As shown in fig. 5b, the metal nanoparticles uniformly distributed on the surface of the substrate and the carbon nanotubes form a stable state after high-temperature annealing, so that the adhesion force of the contact between the carbon nanotubes and the substrate is enhanced, the electron transmission rate on the surface of the carbon nanotubes and the ohmic contact between the substrate and the carbon nanotubes can be effectively improved, the thermal resistance is reduced, and the emission barrier is reduced.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (5)
1. A method of making an ion neutralizer device, comprising the steps of:
(1) sequentially manufacturing a graphical buffer layer and a graphical catalytic layer on the surface of a cathode substrate (101) from bottom to top, and growing a carbon nanotube array (201) on the catalytic layer by a thermal chemical vapor deposition method;
(2) depositing a metal thin layer (202) on the surface of the carbon nano tube array (201) by adopting atomic layer deposition, and forming uniformly dispersed metal nano particles (203) on the surface of the carbon nano tube array (201) through annealing treatment to obtain a carbon nano tube array (201) cathode uniformly modified by the metal nano particles (203);
(3) manufacturing a hollowed-out grid structure by a photoetching process, and depositing a uniformly-coated conducting layer on the surface of the hollowed-out grid structure by adopting atomic layer deposition to obtain a metal grid electrode (401);
(4) encapsulate carbon nanotube array (201) negative pole and metal grid net electrode (401) through insulating layer (301), insulating layer (301) are located negative pole substrate (101) surface, insulating layer (301) are hollow, carbon nanotube array (201) negative pole that metal nanoparticle (203) were evenly decorated is located insulating layer (301) hollow portion, carbon nanotube's array (201) and the fretwork position of grid net structure are aimed at, form sandwich structure, ensure that array (201) negative pole, metal grid net electrode (401) and insulating layer (301) three of carbon nanotube do not conduct each other.
2. The method of manufacturing an ion neutralizer device according to claim 1, wherein the step (4) specifically comprises the steps of:
respectively cutting the cathode of the carbon nanotube array (201), the insulating layer (301) and the metal grid electrode (401) to obtain a discrete cathode unit of the carbon nanotube array (201), and the insulating layer (301) and the metal grid electrode (401) which correspond to the discrete cathode unit of the carbon nanotube array;
the cathode unit of the carbon nanotube array (201) and the insulating layer (301) are connected in an aligning way to ensure that the cathode unit and the insulating layer are not conducted;
and connecting the metal grid electrode (401) with the insulating layer (301) connected with the cathode unit of the carbon nanotube array (201), and ensuring that the cathode unit of the carbon nanotube array (201) is aligned with the hollow position of the grid structure.
3. The method of manufacturing an ion neutralizer device according to claim 1, wherein the step (4) specifically comprises the steps of:
aligning the cathode of the carbon nanotube array (201) and the insulating layer (301), and connecting the cathode and the insulating layer in a wafer bonding mode to ensure that the cathode and the insulating layer are not conducted;
connecting a metal grid electrode (401) with an insulating layer (301) connected with the cathode of the carbon nanotube array (201) in a wafer bonding mode, and ensuring that the cathode unit of the carbon nanotube array (201) is aligned with the hollowed-out position of the grid structure to form a sandwich structure;
and cutting the wafer to obtain the discrete ion neutralizer.
4. The method for preparing an ion neutralizer device according to any one of claims 1 to 3, wherein the cathode substrate (101) is subjected to a cleaning pretreatment before the patterned buffer layer and the catalytic layer are sequentially formed on the surface of the cathode substrate (101) from bottom to top.
5. The method of any one of claims 1 to 3, wherein the grid substrate is pre-treated by cleaning before the hollowed-out grid structure is fabricated by photolithography.
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