CN111501018B - Method for improving coating gain stability of MCP channel by using ALD (atomic layer deposition) method, ALD-MCP and application - Google Patents
Method for improving coating gain stability of MCP channel by using ALD (atomic layer deposition) method, ALD-MCP and application Download PDFInfo
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- CN111501018B CN111501018B CN202010388763.3A CN202010388763A CN111501018B CN 111501018 B CN111501018 B CN 111501018B CN 202010388763 A CN202010388763 A CN 202010388763A CN 111501018 B CN111501018 B CN 111501018B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45527—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/403—Oxides of aluminium, magnesium or beryllium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J43/00—Secondary-emission tubes; Electron-multiplier tubes
- H01J43/04—Electron multipliers
- H01J43/06—Electrode arrangements
- H01J43/18—Electrode arrangements using essentially more than one dynode
- H01J43/24—Dynodes having potential gradient along their surfaces
- H01J43/246—Microchannel plates [MCP]
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- 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
- H01J9/02—Manufacture of electrodes or electrode systems
Abstract
The invention relates to the technical field of MCP, and provides a method for improving the gain stability of an MCP channel coating film by using ALD, ALD-MCP and application. The invention utilizes ALD technology to deposit Al on the basis of the functional layer of the microchannel plate2O3Before the film layer, a pretreatment layer is firstly manufactured to realize Al2O3Transition between the film layer and the MCP substrate silicon-rich layer; then depositing Al by ALD technique on the basis of the pretreatment layer2O3And (5) film layer. Thus, Al is deposited as ALD through a pretreatment layer2O3The transition between the film layer and the MCP substrate silicon-rich layer avoids forming interface defect charges and improves the ALD-MCP gain stability.
Description
Technical Field
The invention relates to the technical field of microchannel plates, in particular to a method for improving the coating gain stability of an MCP channel by using ALD (atomic layer deposition), which solves the problem of unstable gain of a novel ALD-MCP prepared on the basis of a conventional microchannel plate (MCP) by using the ALD technology.
Background
The Microchannel Plate (MCP) is composed of a plurality of (10)4～107) A compact two-dimensional array of Channel Electron Multipliers (CEM), each channel being a channel electron multiplier with a functional layer on the inner wall that emits secondary electrons. When the MCP is in a working state, a certain voltage (hundreds to thousands of volts) is applied to two ends, an electric field distributed along the axial direction of the channel is formed in the channel, external low-energy particles (electrons, ions or photons) entering the microchannel plate collide with the wall at a certain energy and angle to excite and generate secondary electrons, the secondary electrons accelerate to advance along the channel to the direction of the output end of the MCP along a parabolic path under the action of the electric field force, and collide with the channel wall again in the process to generate more new secondary electrons, so that multiple cascade multiplication is formed, and finally a large number of electrons are emitted at the output end to realize the electron multiplication function. The MCP has the advantages of small size, light weight, high gain, low noise, good uniformity, high spatial resolution, fast time response and the like, and is widely applied to the fields of night vision technology, space technology, optoelectronics, radiation detection instruments and the like.
The traditional MCP is prepared by manufacturing a silicate leather material glass tube containing lead and bismuth and an acid-soluble core material glass rod, performing processes of wire drawing, screen arrangement, hot melt pressing, slicing, coarse grinding, polishing, corrosion, hydrogen reduction, film coating and the like twice, and forming a qualified product after inspection and testing. In the manufacturing process of the traditional MCP, the cladding glass is required to have good thermal stability and chemical stability, a functional layer with conductive capability and secondary electron emission capability can be formed on the surface layer of the inner wall of a channel after hydrogen burning treatment, and meanwhile, the matching with the core glass is also required to be considered in the aspects of softening temperature, viscosity and the like, so that the limited factors are more. By adjusting the component proportion of the glass and optimizing the preparation process, the improvement of the performance such as gain, service life and the like of the traditional MCP has a plurality of limitations, great difficulty and non-ideal effect.
In order to obtain MCPs with high performance parameters, such as high gain, low dark count, long lifetime, researchers have turned their eyes to a new fabrication technique, the atomic layer deposition fabrication technique. Atomic Layer Deposition (ALD) is a special chemical vapor deposition method that forms deposited films by alternately pulsing vapor phase precursors into a reaction chamber and chemisorbing and reacting on a substrate, the reaction being self-limiting, i.e., the reaction is automatically terminated when one precursor is saturated with another. The self-limiting characteristic of atomic layer growth enables the prepared film to have the characteristics of accurate and controllable thickness, good surface uniformity, excellent shape retention and the like, and is widely applied to scientific research and commercial production at present. The technology can deposit a functional film layer with a high secondary electron emission coefficient in the groove and the channel with a high depth-to-width ratio, removes the limitation of the traditional preparation technology on the MCP performance, brings certain possibility for improving the performance of the microchannel plate, and has the advantages of getting attention of a plurality of scientific researchers in recent years and wide development prospect.
In the case of ALD-MCP, the most commonly used material for the membrane layer is alumina. One of the most desirable ALD reactions is the reaction of Trimethylaluminum (TMA) with water as a precursor to alumina, the reaction equation being as follows:
AlOH*+Al(CH3)3→AlOAl(CH3)2*+CH4 (1)
Al(CH3)2*+H2O→Al(OH)*+CH4 (2)
in the prior art, ALD-MCP prepared by preparing an alumina film layer on the traditional MCP has very obvious improvement in gain and service life, but has certain problems correspondingly: the ALD-MCP has the condition of unstable gain, the gain is increased along with the increase of working time during initial working in a vacuum device, the gain rise amplitude of a single-chip microchannel plate exceeds 50%, the superimposed gain rise amplitude of a double-chip microchannel plate also exceeds 30%, and the gain stable state can be achieved after a long period of working, and the phenomenon is also called as positive memory effect in imaging application. Related experiments were also conducted by the prior art Photonis and the company Photek, and the results of the tests by the company Photonis and the company Photek shown in fig. 1 and 2 show that the gains of the tests by the company Photonis and the company Photek are in an unstable state.
Disclosure of Invention
The invention aims to provide a method for improving the gain stability of an MCP channel coating by using ALD (atomic layer deposition), which comprises the steps of pretreating an MCP substrate to form a pretreatment layer, and depositing Al with a high secondary electron emission coefficient by using the ALD technology2O3The film material and the ALD-MCP manufactured by the method can obtain better gain stability in the use process.
In the prior art, ALD-MCP is generally used for preparing a film material with a high secondary electron emission coefficient uniformly penetrating the thickness of a channel film in a channel by using an atomic layer deposition technology based on conventional MCP, such as Al2O3The film material has good stability and environmental adaptability. Direct deposition of Al as used in the prior art2O3The situation that the gain is unstable can occur when the ALD-MCP is used by the film material, the gain can be increased along with the extension of the working time when the ALD-MCP works in a vacuum device, the gain rising amplitude of a single-chip microchannel plate exceeds 50%, the superimposed gain rising amplitude of a double-chip microchannel plate also exceeds 30%, and the stable gain state can be achieved after a long period of working.
The ALD-MCP gain of the deposited aluminum oxide film material is unstable and is related to interface defect charges between the film layer and the MCP substrate. Silicon-rich layer of MCP substrate surface is made of SiO2Mainly in SiO2Surface deposition of Al directly using ALD2O3Film layer, interface defect charge is generated at the interface, SiO2One side of which forms positive defect charges in Al2O3One side forms negative defect charges, so that an electric field with certain strength is formed in a certain range at the interface and the periphery. During the operation of the ALD-MCP, charges need to be continuously extracted from the substrate as a supplement after the emission of secondary electrons, and when the supplementary electrons pass through the interface, the distribution of the interface charges is affected, so that the disturbance of an electric field is caused, the supplement of electrons and the emission of the secondary electrons are affected, and the instability of gain is caused.
In order to solve the problem, the invention provides a method for improving the gain stability of the coating of an MCP channel by using ALD (atomic layer deposition), and Al is deposited on the ALD2O3Before the film layer, a pretreatment layer is firstly manufactured to realize the method for improving the gain stability. The pretreatment layer can be used for ALD deposition of Al2O3The transition between the film layer and the MCP substrate silicon-rich layer avoids forming interface defect charges and solves the problem of unstable gain of the ALD-MCP.
Further, the material of the pretreatment layer is chromium oxide (Cr)2O3)。
Furthermore, the chromium oxide film layer is of a nano-particle structure, the size of nano-particles is between 0.5nm and 20nm, and the overall thickness of the formed film layer is between 1nm and 20 nm.
Further, the chromic oxide nano particles are dispersed in the water/ethanol mixed solution by using ultrasonic waves to form uniform mixed solution, the microchannel plate is placed in the water/ethanol mixed solution, the mixed solution can completely enter the microchannel plate by using an ultrasonic method, the microchannel plate is taken out, redundant mixed solution is removed, and drying is carried out, so that the nano particles can be attached to the inner wall of the channel to form a uniform film layer consisting of the nano particles.
Furthermore, the thickness range of the film layer is controlled by controlling the proportion of water, ethanol and nano particles in the mixed solution.
Further, on the pretreated MCP substrate, Al is deposited on the inner wall of the channel by using trimethyl aluminum and water as precursors through an ALD (atomic layer deposition) technology2O3The thickness of the film layer is 1nm-15 nm.
Furthermore, the ALD-MCP can be used in micro-optical image enhancement in a single chip mode or used in a detector of a weak signal in a mode of double-chip V-shaped superposition and three-chip Z-shaped superposition.
It should be understood that all combinations of the foregoing concepts and additional concepts described in greater detail below can be considered as part of the inventive subject matter of this disclosure unless such concepts are mutually inconsistent. In addition, all combinations of claimed subject matter are considered a part of the presently disclosed subject matter.
The foregoing and other aspects, embodiments and features of the present teachings can be more fully understood from the following description taken in conjunction with the accompanying drawings. Additional aspects of the present invention, such as features and/or advantages of exemplary embodiments, will be apparent from the description which follows, or may be learned by practice of specific embodiments in accordance with the teachings of the present invention.
Drawings
The drawings are not intended to be drawn to scale. In the drawings, each identical or nearly identical component that is illustrated in various figures may be represented by a like numeral. For purposes of clarity, not every component may be labeled in every drawing. Embodiments of various aspects of the present invention will now be described, by way of example, with reference to the accompanying drawings, in which:
FIG. 1 is a graph showing the results of a prior art gain test by Photonics corporation.
FIG. 2 is a graph showing the results of a prior art gain test by Photek.
FIG. 3 is a schematic diagram of the structure of the film layer of the ALD-MCP prepared by the invention.
FIG. 4 is a schematic diagram of the structural effect of adding a pretreatment layer according to the present invention.
FIG. 5 is a graph showing a comparison of gain stability before and after the technique of the present invention is used
Description of reference numerals:
1-microchannel plate base; 2-functional area of inner wall surface of channel; 3-ALD depositing an Al2O3 film layer; 4-pretreatment layer; 5-emitting layer (silicon rich layer); 6-a transition layer; 7-a conductive layer; 8-ALD depositing an Al2O3 film layer; 9-pretreatment layer; 10-a silicon dioxide layer; 11-ALD-MCP gain test without pretreatment layer; 12-ALD-MCP gain test with pretreatment layer; 13-without ALD conventional MCP.
Detailed Description
In order to better understand the technical content of the present invention, specific embodiments are described below with reference to the accompanying drawings.
In this disclosure, aspects of the present invention are described with reference to the accompanying drawings, in which a number of illustrative embodiments are shown. Embodiments of the present disclosure are not necessarily intended to include all aspects of the invention. It should be appreciated that the various concepts and embodiments described above, as well as those described in greater detail below, may be implemented in any of numerous ways, as the disclosed concepts and embodiments are not limited to any one implementation. In addition, some aspects of the present disclosure may be used alone, or in any suitable combination with other aspects of the present disclosure.
Referring to fig. 3-4, an exemplary embodiment of the present invention provides a method for improving gain stability of MCP channel coating using ALD, which is to deposit Al using ALD2O3Before the film layer, a pretreatment layer is made. In a specific operation, as shown in fig. 1, on the basis of the functional layer of MCP, a pretreatment layer for achieving a transition on the silicon-rich layer of the functional layer is first prepared, and then Al is deposited on the basis of the pretreatment layer2O3Film layer such that the pretreatment layer deposits Al as ALD2O3The transition between the film layer and the MCP substrate silicon-rich layer avoids forming interface defect charges and solves the problem of unstable gain of the ALD-MCP.
Preferably, the material of the pretreatment layer is chromium oxide (Cr)2O3). Particularly, the chromium oxide pretreatment layer is of a nano-particle structure, the size of nano-particles is between 0.5nm and 20nm, and the overall thickness of the formed film layer is between 1nm and 20 nm.
Further, in the preparation process, the chromic oxide nano particles are dispersed in the water/ethanol mixed solution by using ultrasonic waves to form uniform mixed solution, the microchannel plate is placed in the water/ethanol mixed solution, the mixed solution can completely enter the microchannel plate by using an ultrasonic method, the microchannel plate is taken out, redundant mixed solution is removed, drying is carried out, the nano particles can be attached to the inner wall of the channel, and a film layer consisting of uniform nano particles is formed. The reaction time is between 30 and 120s, ensuring sufficient adhesion and uniformity. Meanwhile, the reaction time is controlled within 120s in order to ensure the uniformity and the thickness of the film layer.
The reaction time was 120s, as described in the examples below.
Wherein, in the preparation process, the thickness range of the film layer is controlled by controlling the proportion of water, ethanol and nano particles in the mixed solution.
Further, on the pretreated MCP substrate, trimethyl aluminum and water are used as precursors, and Al is deposited on the inner wall of the channel of the microchannel plate through an ALD (atomic layer deposition) technology2O3The thickness of the film layer is controlled within the range of 1nm-15nm, so that the high-gain stable microchannel plate structure is manufactured.
In alternative embodiments, the ALD-MCP prepared by the process of the present invention can be used in a micro-optical image intensifier device in a single chip or in a detector of a weak signal in a mode of double-chip V-shaped superposition and three-chip Z-shaped superposition
The foregoing manufacturing process is described in more detail below with reference to specific examples.
In the examples of the present invention, ALD-MCP with a pretreatment layer was prepared using the method of the present invention, and then comparison was performed using ALD-MCP without a pretreatment layer.
Wherein, the preparation process of the ALD-MCP with the pretreatment layer according to the scheme of the invention comprises the following steps:
(1) taking 2 g of chromic oxide nano particles (the particle size is 2nm-4nm), putting the chromic oxide nano particles into 100ml of water/ethanol mixed solution (the volume ratio is 1:1), stirring, and forming uniform mixed solution by using an ultrasonic dispersion mode;
(2) putting the micro-channel plate into a micro-channel plate, performing ultrasonic treatment for 2min, immediately taking out the micro-channel plate, putting the micro-channel plate into a vacuum oven at the temperature of 200 ℃, performing vacuum-pumping drying, and performing heat preservation for 2h to prepare a pretreatment layer with the thickness of 4 nm;
(3) preparing an MCP substrate with the pre-treatment layer, putting the MCP substrate into an ALD reaction chamber, and preparing Al2O3The film adopts the following process: TMA/N2/H2O/N22s/1min/2s/1min, the deposition temperature is 240 ℃, and the cycle number is 80 (-8 nm).
The MCP without the pretreatment layer is directly prepared by the step (3).
It should be understood that in a specific manufacturing process, according to the teachings of the present invention, for the above-described manufacturing process of ALD-MCP with a pretreatment layer, the process parameters can be appropriately adjusted by those skilled in the art as needed to manufacture suitable and different ALD-MCPs.
With reference to fig. 4 and 5, the ALD-MCP without the pretreatment layer and the ALD-MCP without the pretreatment layer are prepared, and a two-chip stacking test method is adopted to test the fluctuation condition of the gain, and as a result, as shown in fig. 5, the maximum increase amount of the ALD-MCP without the pretreatment layer reaches more than 30%, and the variation amount of the ALD-MCP gain with the pretreatment layer is less than 5%.
Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention. Therefore, the protection scope of the present invention should be determined by the appended claims.
Claims (8)
1. A method for improving the gain stability of an MCP channel coating by using ALD (atomic layer deposition), which is characterized by comprising the following steps:
depositing Al on the basis of functional layers of a microchannel plate by using an ALD (atomic layer deposition) technology2O3Before the film layer, a pretreatment layer is firstly manufactured to realize Al2O3Transition between the film layer and the MCP substrate silicon-rich layer; then depositing Al by ALD technique on the basis of the pretreatment layer2O3A film layer;
wherein the material of the pretreatment layer is chromium oxide (Cr)2O3）；
The chromium sesquioxide pretreatment layer is of a nano-particle structure, the size of nano-particles is between 0.5nm and 20nm, and the overall thickness of a formed film layer is between 1nm and 20 nm.
2. A method for improving gain stability of MCP channel coating using ALD according to claim 1, wherein the preparation of the pretreatment layer comprises:
dispersing chromium oxide nano particles in a water/ethanol mixed solution by using ultrasonic waves to form a uniform mixed solution;
placing the microchannel plate into the mixed liquid, enabling the mixed liquid to enter the microchannel plate through ultrasonic vibration to carry out particle attachment, taking out the microchannel plate after attaching for a period of time, removing redundant mixed liquid, and then carrying out drying treatment under a vacuum environment to enable the nano particles to be attached to the inner wall of the channel to form a uniform pretreatment layer consisting of chromium oxide nano particles.
3. The method of improving the gain stability of the coating of the MCP channel by the ALD method as claimed in claim 2, wherein the thickness range of the film layer is controlled by controlling the proportion of the water, the ethanol and the nanoparticles in the mixed solution.
4. A method for improving gain stability of an MCP channel coating using ALD according to claim 2 or 3, wherein the attachment reaction time of the microchannel plate in the mixed liquid is 30-120 s.
5. A method for improving the gain stability of MCP channel coating by ALD as claimed in claim 1, characterized in that on the basis of the pretreatment layer, Al is deposited on the inner wall of the channel by ALD technique using trimethylaluminum and water as precursors2O3The thickness of the film layer is 1nm-15 nm.
6. ALD-MCP prepared according to the method of any one of claims 1 to 5.
7. Use of the ALD-MCP of claim 6 in a micro-optical image intensifier device, comprising a sheet of the ALD-MCP.
8. Use of the ALD-MCP in a weak signal detector according to claim 6, wherein two ALD-MCPs are used in a V-shaped stacked arrangement, or three ALD-MCPs are used in a Z-shaped stacked arrangement.
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| CN103789730A (en) * | 2014-01-16 | 2014-05-14 | 西安交通大学 | Preparation method of secondary-electron emission thin film |
| CN105385997A (en) * | 2015-11-06 | 2016-03-09 | 北京有色金属研究总院 | Cr2O3 film system and preparing method thereof |
| CN106637079A (en) * | 2016-12-02 | 2017-05-10 | 西安交通大学 | Buffer layer of secondary electron emission film and preparation method thereof |
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| CN103789730A (en) * | 2014-01-16 | 2014-05-14 | 西安交通大学 | Preparation method of secondary-electron emission thin film |
| CN105385997A (en) * | 2015-11-06 | 2016-03-09 | 北京有色金属研究总院 | Cr2O3 film system and preparing method thereof |
| CN106637079A (en) * | 2016-12-02 | 2017-05-10 | 西安交通大学 | Buffer layer of secondary electron emission film and preparation method thereof |
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